830-13-7|Cyclododecanone| Ambeed

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CAS No. :	830-13-7
Formula :	C₁₂H₂₂O
M.W :	182.30
SMILES Code :	O=C1CCCCCCCCCCC1
MDL No. :	MFCD00003722
InChI Key :	SXVPOSFURRDKBO-UHFFFAOYSA-N
Pubchem ID :	13246

GHS Pictogram:
Signal Word:	Danger
Hazard Statements:	H302-H361-H372-H410
Precautionary Statements:	P201-P264-P280-P301+P330+P331-P312
Class:	9
UN#:	3077
Packing Group:	Ⅲ

Yield	Reaction Conditions	Operation in experiment
75.4%		In a 500 ml glass reaction vessel,258.14 g (2.74 mol) of phenol,And 13.73 g (0.137 mol) of 98% sulfuric acid were charged,The temperature was raised to 80 C. After stirring at the same temperature for 1 hour,It was cooled to 60 C.,50.02 g (0.274 mol) of cyclododecanone,5.57 g (0.0275 mol) of n-dodecylmercaptan was charged and stirred for 8 hours at 64 to 68 C. under reduced pressure of 2.7 kPa while blowing nitrogen gas. After completion of stirring, the mixture was allowed to stand still overnight,When the reaction mass was analyzed by gas chromatography,No cyclododecanone was detected. To the resulting reaction mass were added toluene,Ion exchanged water was added and neutralized with sodium hydroxide,Ion exchangeIt was washed with water. The obtained organic layer was cooled as it was,Precipitated crystals were taken out by filtration. The obtained crystals were recrystallized from methanol water, taken out by filtration,After drying, 72.89 g of 1,1-bis (4-hydroxyphenyl) cyclododecane was obtained (HPLC purity 100%, yield 75.4%).
77.04 g		258.19 g (2.74 mol) of phenol and 13.72 g (0.137 mol) of 98% sulfuric acid were charged into a 500 ml glass reaction vessel equipped with a stirrer, a condenser and a thermometer, and the temperature was raised to 80 C. After stirring at the same temperature for 1 hour, 50.09 g (0.275 mol) of cyclododecanone at 60 C.,5.54 g (0.0274 mol) of n-dodecylmercaptan was added and reacted at 65 C. while removing water at 1.3 kPa until the remaining amount of cyclododecanone reached 50% of the initial charge amount.After recovering pressure to normal pressure with nitrogen gas, it was cooled to 30 C. and left to stand at the same temperature for 52 hours.0.15 g of the solidified reaction mass was scraped off, and the reaction mass was analyzed by gas chromatography. As a result, the remaining amount of cyclododecanone was 1% of the initially charged amount, and 1, 1-bis (4-hydroxy Phenyl) cyclododecane (the molar ratio to the initially charged amount of cyclododecanone) was 90.2%. Toluene and ion exchanged water were added to the obtained reaction mass, neutralized with sodium hydroxide, and then washed with ion exchanged water. The obtained organic layer was cooled as it was, the precipitated crystal was taken out by filtration and dried. The obtained crystals were recrystallized from methanol water, taken out by filtration and dried to obtain 77.04 g (0.219 mol, yield 79.5 mmol) of 1, 1-bis (4-hydroxyphenyl) cyclododecane %, HPLC purity 100%) was obtained

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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.
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P370 + P378	In case of fire:
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P401
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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.: 830-13-7

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CAS No.: 830-13-7

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[ 830-13-7 ] Synthesis Path-Downstream 1~4

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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