835633-47-1|1-Bromo-2-(difluoromethoxy)-4-nitrobenzene| Ambeed

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CAS No. :	835633-47-1
Formula :	C₇H₄BrF₂NO₃
M.W :	268.01
SMILES Code :	O=[N+](C1=CC=C(Br)C(OC(F)F)=C1)[O-]
MDL No. :	MFCD15526849
InChI Key :	JFFPRVLUZCLWSF-UHFFFAOYSA-N
Pubchem ID :	53415904

GHS Pictogram:
Signal Word:	Warning
Hazard Statements:	H302-H312-H315-H319-H332-H335
Precautionary Statements:	P261-P264-P270-P271-P280-P301+P312-P302+P352-P304+P340-P305+P351+P338-P330-P332+P313-P337+P313-P362-P403+P233-P405-P501

Yield	Reaction Conditions	Operation in experiment
99%	With potassium carbonate; In N,N-dimethyl-formamide; at 70℃;Inert atmosphere;	(1006) [00349] Into a 250-mL round-bottom flask, purged and maintained under an inert, atmosphere of nitrogen, was added 2-bromo-5-nitrophenol (4.65 g, 21.3 mmol), ethyl 2-chloro-2,2- difluoroacetate (4.50 g, 28.4 mmol), and potassium carbonate (2.9 g, 21 mmol) followed by DMF (30 mL). The reaction mixture was stirred overnight at 70 °C in an oil bath and then quenched with water (50 mL). The resulting solution was extracted with ethyl acetate (3 x lOOmL), the organic layers combined, dried over anhydrous sodium sulfate filtered, and concentrated in vacuo to afford l-bromo-2-(difluoromethoxy)-4-nitrobenzene as a red oil (5.68 g, 99percent), LCMS (ESI, m/z): 268 i'M-H] .
75%	With potassium carbonate; In N,N-dimethyl-formamide; at 70℃; for 5h;Inert atmosphere;	A suspension of 2?bromo?5?nitrophenol (1.00 g, 4.59 mmol), <strong>[383-62-0]ethyl chlorodifluoroacetate</strong> (0.581 mL, 4.59 mmol) and potassium carbonate (0.634 g, 4.59 mmol) in anhydrous DMF (10.35 mL) was heated to 70 °C under a nitrogenatmosphere for 5 hours. The reaction mixture was allowed to cool to room temperature, diluted with water (50 mL) and extracted into ethyl acetate (3 x 25 mL) . The combined organic phases were washed with 50:50 water:brine (3 x 30 mL), dried over Na2504, filtered andconcentrated to dryness under reduced pressure. The residue was purified by Biotage chromatography (silica 50g cartridge, cyclohexane: ethyl acetate, gradient elution from 100:0 to 80:20) to give the title compound as a colourless oil (920 mg, 75percent) . ?H NMR (400 MHz, DMSO?d6) : 3 8.10 (d, 1H), 8.00 (dd, 1H), 7.83 (d, 1H), 6.66 (t,1H)
	With potassium carbonate; In DMF (N,N-dimethyl-formamide); at 70℃; for 5h;	To a N2 purged round bottom flask was added 2-bromo-5- nitrophenol (29.0 g, 133 mmol, 1.0 eq. ) followed by 16.8 mL (133 mmol, 1.0 eq) of <strong>[383-62-0]ethyl chlorodifluoroacetate</strong> and 18. 8 g of K2CO3 (133 MMOL, 1.0 eq. ). Anhydrous DMF (300 mL) was added and the mixture was stirred at 70 °C for 5 h. The mixture was cooled to RT and the solvent was removed. The obtained crude mixture was dissolved in CH2C12 (500 mL) and washed with IN NaOH (aq. ). The organic layer was dried (MGSO4), filtered and evaporated. The crude material was further purified by column chromatography (0-5percent EtOAc in hexanes) providing pure 1-bromo-2-difluoromethoxy-4-nitro- benzene.

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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.
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P401
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Disposal
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P501	Dispose of contents/container to ...
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CAS No.: 835633-47-1

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CAS No.: 835633-47-1

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[ 835633-47-1 ] 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