65060-93-7|3-Bromo-1-methyl-1H-pyrrole-2,5-dione| Ambeed

GHS Pictogram:
Signal Word:	Warning
Hazard Statements:	H315-H319-H335
Precautionary Statements:	P261-P264-P271-P280-P302+P352-P304+P340-P305+P351+P338-P312-P362-P403+P233-P501

Yield	Reaction Conditions	Operation in experiment
73%		Example VIII Preparation of l-Aryl-3-methyl-3-aza-bicyclo[3.1.0]hexane hydrochlorides Using Reaction Scheme 14 A. Synthesis of 3-Bromo-l-methyl-12?-pyitauole-2.,5-dione Pursuant to steps a and b of Reaction Scheme 14, a solution of <strong>[5926-51-2]bromomaleic anhydride</strong> (52.8 g, 0.298 mol) in diethyl ether (250 mL) was cooled to 5 0C. A 2 M solution of methylamine in TEtaF (298 mL, 0.596 mol, 2 eq.) was added dropwise EPO <DP n="86"/>over 1 hour and the reaction stirred for a further 30 minutes, maintaining the temperature below 10 0C. The resulting precipitate was filtered, washed with diethyl ether (2 x 100 mL) and air-dried for 30 minutes, then suspended in acetic anhydride (368 mL) and sodium acetate (12.2 g, 0.149 mol, 0.5 eq.) added. The reaction was heated to 60 0C for 2 hours and solvent was then removed in vacuo. The residue was taken up in DCM (500 mL) and washed with saturated sodium bicarbonate solution (2 x 500 mL) and water (2 x 300 mL). Organics were dried over MgSO4 (89 g), filtered and reduced in vacuo. The resulting oil was azeotroped with toluene (4 x 100 mL) to give N-methyl bromomaleimide as a beige solid. Yield = 41.4 g (73 percent); 1H NMR (300 MHz, CDCl3) delta 6.95 (IH, s, CH), 3.07 (3H, s, NCH3).
73%		Example IX; Preparation of l-Aryl-3-methyl-3-aza-bicyclof3.1.0]hexane hydrochloridesUsing Reaction Scheme 14A. Synthesis of 3-Bromo-l-methyl-ljH-pyrrole-2.,5-dionePursuant to steps a and b of Reaction Scheme 14, a solution of <strong>[5926-51-2]bromomaleic anhydride</strong> (52.8 g, 0.298 mol) in diethyl ether (250 mL) was cooled to 5 0C. A 2 M solution of methylamine in THF (298 mL, 0.596 mol, 2 eq.) was added dropwise over 1 hour and the reaction stirred for a further 30 minutes, maintaining the temperature below 10 °C. The resulting precipitate was filtered, washed with diethyl ether (2 x 100 mL) and air-dried for 30 minutes then suspended in acetic anhydride (368 mL) and sodium acetate (12.2 g, 0.149 mol, 0.5 eq.) added. The reaction was heated to 60 °C for 2 hours and then solvent was removed in vacuo. The residue was taken up in DCM (500 mL) and washed with saturated sodium bicarbonate solution (2 x 500 mL) and water (2 x 300 mL). Organics were dried over MgSO4 (89 g), filtered and reduced in vacuo. The resulting oil was azeotroped with toluene (4 x 100 mL) to give N-methyl bromomaleimide as a beige solid. Yield = 41.4 g (73 percent); 1H NMR (300 MHz, CDCl3) delta 6.95 (IH, s, CH), 3.07 (3Eta, s, NCH3)
73%	In tetrahydrofuran; diethyl ether; at 5 - 10℃; for 1.5h;	A solution of <strong>[5926-51-2]bromomaleic anhydride</strong> (aldrich) (52.8 g, 0.298 mol) in diethyl ether (250 mL) was cooled to 5 0C. A 2 M solution of methylamine in THF (298 mL, 0.596 mol, 2 eq.) was added dropwise over 1 hour and the reaction stirred for a further 30 minutes, maintaining the temperature below 10 0C. The resulting precipitate was filtered, washed with diethyl ether (2 x 100 mL) and air-dried for 30 minutes then suspended in acetic anhydride (368 mL) and sodium acetate (12.2 g, 0.149 mol, 0.5 eq.) added. The reaction was heated to 60 °C for 2 hours then solvent removed in vacuo. The residue was taken up in DCM (500 mL) and washed with saturated sodium bicarbonate solution (2 x 500 mL) and water (2 x 300 mL). Organics were dried over MgSO4 (89 g), filtered and reduced in vacuo. The resulting oil was azeotroped with toluene (4 x 100 mL) to give N- methyl bromomaleimide as a beige solid (41.4 g, 73 percent); 1H NMR (300 MHz, CDCl3) delta 6.95 (IH, s, CH), 3.07 (3Eta, s, CH3N).

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3-Bromo-1-methyl-1H-pyrrole-2,5-dione

CAS No.: 65060-93-7

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[ 65060-93-7 ] 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