2754-32-7|1,4-Phenylenebis(dimethylsilanol)| Ambeed

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CAS No. :	2754-32-7
Formula :	C₁₀H₁₈O₂Si₂
M.W :	226.42
SMILES Code :	O[Si](C1=CC=C([Si](C)(C)O)C=C1)(C)C
MDL No. :	MFCD00039516
Boiling Point :	No data available
InChI Key :	YBNBOGKRCOCJHH-UHFFFAOYSA-N
Pubchem ID :	75989

GHS Pictogram:
Signal Word:	Warning
Hazard Statements:	H315-H319-H335
Precautionary Statements:	P261-P305+P351+P338

Yield	Reaction Conditions	Operation in experiment
92%		A double-necked round-bottom flask was set up with a reaction device on which a reflux tube was placed, and the inside was dried and removed, and replaced with a nitrogen atmosphere. Measure the pre-dried anhydrous methanol (250 ml) into a reaction device and place the reaction device in an ice water bath. Under a nitrogen or argon atmosphere, 6.3 g (274.2 mmol) of sodium metal cut into small pieces was carefully added successively. After the metal sodium had completely reacted with methanol and no hydrogen bubbles were generated, a first solution of sodium methoxide was prepared. Weighing 17.8 g (91.4 millimoles) of dioxane of structural formula (A-1) in a feeding tube, Pre-dried anhydrous methanol (50 ml) was added to the feed tube to prepare a bis-decane solution of structural formula (A-1), which was the second solution. The rate of dropwise addition was controlled and the second solution was slowly fed into the first solution in the reaction apparatus. Hydrogen bubbles continued to be generated during the addition. After the dropwise addition was completed, stirring was continued at room temperature for 10 minutes until the generation of hydrogen gas was moderated until it subsided, which was the third solution. Then, a mixed solution of 11.0 g (274.2 millimoles) and water (150 ml) of pre-formulated sodium hydroxide was slowly added dropwise to the third solution, and stirring was continued at room temperature for 20 minutes. This is the fourth solution, and the hydrolysis reaction has been completed so far. After the reaction was completed, a saturated aqueous solution of ammonium chloride was gradually added to the fourth solution for neutralization, and the mixture was cooled in an ice-water bath and stirred for 20 minutes. This was the fifth solution. The fifth solution was transferred to a separatory funnel and extracted with ether (200 ml/3 times). The organic layer was collected and washed with saturated brine (300 ml), dried over anhydrous magnesium sulfate and filtered. The filtrate was concentrated under reduced pressure to give the crude product of the white solid as the phenylephrine of formula (I-1). N-hexane was added to the crude white solid product of the phenylenedioxylanol of formula (I-1). After thorough and uniform mixing, the mixture was collected by suction filtration. The white filter cake was washed with n-hexane, and the white solid product was collected and dried to obtain 19.1 g of the bis-stanol product of formula (I-1). The yield was 92%.
92%		Synthesis of compound (I-1): Setup a reaction device, such as a reflux pipe, on a two-necked round bottom flask. Dry the inside of the two-necked round bottom flask. Introduce nitrogen gas into the two-necked round bottom flask. Put 250 mL of pre-dried anhydrous methanol in the reaction device. Place the reaction device in an ice water bath. Chips of 6.3 g (274.2 mmol) of metallic sodium are put in the reaction device immersed in the ice water bath under nitrogen gas or argon gas atmosphere one by one and carefully. After the metallic sodium has reacted with methanol completely and no hydrogen bubbles have been generated, the first solution of sodium methoxide is produced. Then, 17.8 g (91.4 mmol) of disilane with structural formula (A-1) and 50 mL of pre-dried anhydrous methanol are introduced into the feeding pipe to form a disilane (expressed by structural formula (A-1)) solution known as the second solution. Drip the second solution slowly to the first solution in the reaction device while hydrogen bubbles are being continuously generated. Afterward, the mixture of first and second solutions are stirred for 10 minutes at room temperature while the generation of hydrogen gas is fading out, thereby producing the third solution. Then, an aqueous solution of a mixture of 11.0 g (274.2 mmol) of sodium hydroxide and 150 mL of water is dripped slowly to the third solution while the third solution is being stirred for 20 minutes, so as to produce the fourth solution. At this point in time, the hydrolysis process is finished, and a saturated ammonium chloride aqueous solution is added to the fourth solution to trigger neutralization therebetween while the fourth solution is being cooled and stirred in an ice water bath for 20 minutes to produce the fifth solution. Transfer the fifth solution to a separatory funnel to undergo extraction with 200 mL of ether thrice, and then collect the organic supernatant before rinsing it with 300 mL of saturated brine solution for the sake of drying. A drying process is performed with anhydrous magnesium sulfate, and then filtration is performed so that the filtrate is depressurized and concentrated to obtain a crude white solid product of phenylene disilanol with structural formula (I-1). Add n-hexane to the crude white solid product of phenylene disilanol with structural formula (I-1) and mix them. Collect the solid precipitate by suction filtration. Rinse the white solid with n-hexane. Collect the white solid product and dry it to obtain 19.1 g of disilanol with structural formula (I-1) at a yield of 92%. Referring to FIG. 4, it shows the 1H-NMR spectrum for phenylene disilanol according to an embodiment of the present invention.

Precautionary Statements-General
Code	Phrase
P101	If medical advice is needed,have product container or label at hand.
P102	Keep out of reach of children.
P103	Read label before use
Prevention
Code	Phrase
P201	Obtain special instructions before use.
P202	Do not handle until all safety precautions have been read and understood.
P210	Keep away from heat/sparks/open flames/hot surfaces. - No smoking.
P211	Do not spray on an open flame or other ignition source.
P220	Keep/Store away from clothing/combustible materials.
P221	Take any precaution to avoid mixing with combustibles
P222	Do not allow contact with air.
P223	Keep away from any possible contact with water, because of violent reaction and possible flash fire.
P230	Keep wetted
P231	Handle under inert gas.
P232	Protect from moisture.
P233	Keep container tightly closed.
P234	Keep only in original container.
P235	Keep cool
P240	Ground/bond container and receiving equipment.
P241	Use explosion-proof electrical/ventilating/lighting/equipment.
P242	Use only non-sparking tools.
P243	Take precautionary measures against static discharge.
P244	Keep reduction valves free from grease and oil.
P250	Do not subject to grinding/shock/friction.
P251	Pressurized container: Do not pierce or burn, even after use.
P260	Do not breathe dust/fume/gas/mist/vapours/spray.
P261	Avoid breathing dust/fume/gas/mist/vapours/spray.
P262	Do not get in eyes, on skin, or on clothing.
P263	Avoid contact during pregnancy/while nursing.
P264	Wash hands thoroughly after handling.
P265	Wash skin thouroughly after handling.
P270	Do not eat, drink or smoke when using this product.
P271	Use only outdoors or in a well-ventilated area.
P272	Contaminated work clothing should not be allowed out of the workplace.
P273	Avoid release to the environment.
P280	Wear protective gloves/protective clothing/eye protection/face protection.
P281	Use personal protective equipment as required.
P282	Wear cold insulating gloves/face shield/eye protection.
P283	Wear fire/flame resistant/retardant clothing.
P284	Wear respiratory protection.
P285	In case of inadequate ventilation wear respiratory protection.
P231 + P232	Handle under inert gas. Protect from moisture.
P235 + P410	Keep cool. Protect from sunlight.
Response
Code	Phrase
P301	IF SWALLOWED:
P304	IF INHALED:
P305	IF IN EYES:
P306	IF ON CLOTHING:
P307	IF exposed:
P308	IF exposed or concerned:
P309	IF exposed or if you feel unwell:
P310	Immediately call a POISON CENTER or doctor/physician.
P311	Call a POISON CENTER or doctor/physician.
P312	Call a POISON CENTER or doctor/physician if you feel unwell.
P313	Get medical advice/attention.
P314	Get medical advice/attention if you feel unwell.
P315	Get immediate medical advice/attention.
P320
P302 + P352	IF ON SKIN: wash with plenty of soap and water.
P321
P322
P330	Rinse mouth.
P331	Do NOT induce vomiting.
P332	IF SKIN irritation occurs:
P333	If skin irritation or rash occurs:
P334	Immerse in cool water/wrap n wet bandages.
P335	Brush off loose particles from skin.
P336	Thaw frosted parts with lukewarm water. Do not rub affected area.
P337	If eye irritation persists:
P338	Remove contact lenses, if present and easy to do. Continue rinsing.
P340	Remove victim to fresh air and keep at rest in a position comfortable for breathing.
P341	If breathing is difficult, remove victim to fresh air and keep at rest in a position comfortable for breathing.
P342	If experiencing respiratory symptoms:
P350	Gently wash with plenty of soap and water.
P351	Rinse cautiously with water for several minutes.
P352	Wash with plenty of soap and water.
P353	Rinse skin with water/shower.
P360	Rinse immediately contaminated clothing and skin with plenty of water before removing clothes.
P361	Remove/Take off immediately all contaminated clothing.
P362	Take off contaminated clothing and wash before reuse.
P363	Wash contaminated clothing before reuse.
P370	In case of fire:
P371	In case of major fire and large quantities:
P372	Explosion risk in case of fire.
P373	DO NOT fight fire when fire reaches explosives.
P374	Fight fire with normal precautions from a reasonable distance.
P376	Stop leak if safe to do so. Oxidising gases (section 2.4) 1
P377	Leaking gas fire: Do not extinguish, unless leak can be stopped safely.
P378
P380	Evacuate area.
P381	Eliminate all ignition sources if safe to do so.
P390	Absorb spillage to prevent material damage.
P391	Collect spillage. Hazardous to the aquatic environment
P301 + P310	IF SWALLOWED: Immediately call a POISON CENTER or doctor/physician.
P301 + P312	IF SWALLOWED: call a POISON CENTER or doctor/physician IF you feel unwell.
P301 + P330 + P331	IF SWALLOWED: Rinse mouth. Do NOT induce vomiting.
P302 + P334	IF ON SKIN: Immerse in cool water/wrap in wet bandages.
P302 + P350	IF ON SKIN: Gently wash with plenty of soap and water.
P303 + P361 + P353	IF ON SKIN (or hair): Remove/Take off Immediately all contaminated clothing. Rinse SKIN with water/shower.
P304 + P312	IF INHALED: Call a POISON CENTER or doctor/physician if you feel unwell.
P304 + P340	IF INHALED: Remove victim to fresh air and Keep at rest in a position comfortable for breathing.
P304 + P341	IF INHALED: If breathing is difficult, remove victim to fresh air and keep at rest in a position comfortable for breathing.
P305 + P351 + P338	IF IN EYES: Rinse cautiously with water for several minutes. Remove contact lenses, if present and easy to do. Continue rinsing.
P306 + P360	IF ON CLOTHING: Rinse Immediately contaminated CLOTHING and SKIN with plenty of water before removing clothes.
P307 + P311	IF exposed: call a POISON CENTER or doctor/physician.
P308 + P313	IF exposed or concerned: Get medical advice/attention.
P309 + P311	IF exposed or if you feel unwell: call a POISON CENTER or doctor/physician.
P332 + P313	IF SKIN irritation occurs: Get medical advice/attention.
P333 + P313	IF SKIN irritation or rash occurs: Get medical advice/attention.
P335 + P334	Brush off loose particles from skin. Immerse in cool water/wrap in wet bandages.
P337 + P313	IF eye irritation persists: Get medical advice/attention.
P342 + P311	IF experiencing respiratory symptoms: call a POISON CENTER or doctor/physician.
P370 + P376	In case of fire: Stop leak if safe to Do so.
P370 + P378	In case of fire:
P370 + P380	In case of fire: Evacuate area.
P370 + P380 + P375	In case of fire: Evacuate area. Fight fire remotely due to the risk of explosion.
P371 + P380 + P375	In case of major fire and large quantities: Evacuate area. Fight fire remotely due to the risk of explosion.
Storage
Code	Phrase
P401
P402	Store in a dry place.
P403	Store in a well-ventilated place.
P404	Store in a closed container.
P405	Store locked up.
P406	Store in corrosive resistant/ container with a resistant inner liner.
P407	Maintain air gap between stacks/pallets.
P410	Protect from sunlight.
P411
P412	Do not expose to temperatures exceeding 50 oC/ 122 oF.
P413
P420	Store away from other materials.
P422
P402 + P404	Store in a dry place. Store in a closed container.
P403 + P233	Store in a well-ventilated place. Keep container tightly closed.
P403 + P235	Store in a well-ventilated place. Keep cool.
P410 + P403	Protect from sunlight. Store in a well-ventilated place.
P410 + P412	Protect from sunlight. Do not expose to temperatures exceeding 50 oC/122oF.
P411 + P235	Keep cool.
Disposal
Code	Phrase
P501	Dispose of contents/container to ...
P502	Refer to manufacturer/supplier for information on recovery/recycling

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CAS No.: 2754-32-7

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CAS No.: 2754-32-7

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[ 2754-32-7 ] Synthesis Path-Downstream 1~2

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Physical hazards
Code	Phrase
H200	Unstable explosive
H201	Explosive; mass explosion hazard
H202	Explosive; severe projection hazard
H203	Explosive; fire, blast or projection hazard
H204	Fire or projection hazard
H205	May mass explode in fire
H220	Extremely flammable gas
H221	Flammable gas
H222	Extremely flammable aerosol
H223	Flammable aerosol
H224	Extremely flammable liquid and vapour
H225	Highly flammable liquid and vapour
H226	Flammable liquid and vapour
H227	Combustible liquid
H228	Flammable solid
H229	Pressurized container: may burst if heated
H230	May react explosively even in the absence of air
H231	May react explosively even in the absence of air at elevated pressure and/or temperature
H240	Heating may cause an explosion
H241	Heating may cause a fire or explosion
H242	Heating may cause a fire
H250	Catches fire spontaneously if exposed to air
H251	Self-heating; may catch fire
H252	Self-heating in large quantities; may catch fire
H260	In contact with water releases flammable gases which may ignite spontaneously
H261	In contact with water releases flammable gas
H270	May cause or intensify fire; oxidizer
H271	May cause fire or explosion; strong oxidizer
H272	May intensify fire; oxidizer
H280	Contains gas under pressure; may explode if heated
H281	Contains refrigerated gas; may cause cryogenic burns or injury
H290	May be corrosive to metals
Health hazards
Code	Phrase
H300	Fatal if swallowed
H301	Toxic if swallowed
H302	Harmful if swallowed
H303	May be harmful if swallowed