1240288-81-6|6-Bromobenzo[b]thiophen-3(2H)-one 1,1-dioxide| Ambeed

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CAS No. :	1240288-81-6
Formula :	C₈H₅BrO₃S
M.W :	261.09
SMILES Code :	O=C(C1=CC=C(Br)C=C12)CS2(=O)=O
MDL No. :	MFCD27942487

GHS Pictogram:
Signal Word:	Warning
Hazard Statements:	H302-H315-H319-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
100%		PREPARATION 746-Bromo-1-benzothiophen-3(2H)-one 1 ,1 -dioxideTo a solution of <strong>[773134-43-3]methyl 4-bromo-2-(methylsulfonyl)benzoate</strong> (774 mg, 2.64 mmol) in anhydrous THF (10 mL) was added NaH (60% in mineral, 11 1 mg, 2.77 mmol). The mixture was stirred at room temperature for 5 hr. The reaction was monitored by LCMS for completion. H2O (1 mL) was added to quench the reaction followed by the addition of aqueous hydrochloric acid (1N, 50 mL) and EtOAc (50 mL). The organic layer was separated, and the water layer was extracted with 2 X EtOAc. The combined organic layers were washed with brine, dried over sodium sulfate, filtered, and concentrated to give the title compound (689 mg, 100%) as a white solid.1H NMR (400 MHz, DMSO-d6) δ ppm 4.62 (s, 2H), 7.92 (d, J=8.34 Hz, 1 H), 8.14 (dd, J=8.21 , 1.14 Hz, 1 H), 8.53 (s, 1 H).
92%	With sodium hydride; In tetrahydrofuran; at 20℃; for 2.0h;	To a stirring solution of compound 1(1.7 g, 5.8 mmol) in dry THF (20 mL) was added NaH (139 mg, 5.8 mmol), then stirred at RT for 2 h. Quenched with water and HC1 (iN, 10 ml), extracted with EtOAc, concentrated under reduced pressure to obtain crude product, which was purified by combiflash (petroleum ether:ethyl acetate = 1:1) to give compound 2 (1.4 g, 92%) as ayellow solid. LC-MS: m/z = 26 1.0/263.0 [M+H]
	With sodium hydride; In tetrahydrofuran; at 20℃; for 1.5h;	A solution of <strong>[773134-43-3]methyl 4-bromo-2-(methylsulfonyl)benzoate</strong> (Intermediate 239; 4.00 g; 13.6 mmol) in anhydrous THF (60 ml) was treated with NaH (595 mg; 13.6 mmol) and stirred at RT for 1.5 h. The reaction was quenched with water. AcOEt and a 1 N solution of HCI in water were added and the phases were separated. The organic phase was washed with brine, dried on MgSO4, filtered and concentrated to give the title compound as a yellow solid (3.63 g).1H NMR (300MHz, DMSO-d6) δ [ppm] 8.55 (1 H, d, J= 1.7 Hz), 8.15 (1 H, d, J= 1.7 Hz, 8.2Hz), 7.93 (1 H, d, J= 8.2 Hz), 4.62 (2H, s). MS (ESI"): 261.0. HPLC (Condition A): Rt 2.56 min.

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Prevention
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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.
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P263	Avoid contact during pregnancy/while nursing.
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P270	Do not eat, drink or smoke when using this product.
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P273	Avoid release to the environment.
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P284	Wear respiratory protection.
P285	In case of inadequate ventilation wear respiratory protection.
P231 + P232	Handle under inert gas. Protect from moisture.
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Code	Phrase
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P342	If experiencing respiratory symptoms:
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P378
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P301 + P312	IF SWALLOWED: call a POISON CENTER or doctor/physician IF you feel unwell.
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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
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P401
P402	Store in a dry place.
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P411
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P422
P402 + P404	Store in a dry place. Store in a closed container.
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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.: 1240288-81-6

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CAS No.: 1240288-81-6

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[ 1240288-81-6 ] Synthesis Path-Downstream 1~1

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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