반응식
[F:1][C:2]1[CH:3]=[CH:4][C:5]([N+:9]([O-:11])=[O:10])=[C:6](N)[CH:7]=1.FC(F)(F)C(OC(=O)C(F)(F)F)=O.FC(F)(F)[C:27]([NH2:29])=O.[OH-].[Na+].S(OC)(OC)(=O)=O>C(Cl)Cl.C1(C)C=CC=CC=1.[Cl-].C([N+](C)(C)C)C1C=CC=CC=1.C(#N)C>[F:1][C:2]1[CH:3]=[CH:4][C:5]([N+:9]([O-:11])=[O:10])=[C:6]([CH2:27][NH2:29])[CH:7]=1참가 물질
반응물 5
생성물 1
시약·촉매·용매 4
반응 조건
- 온도
- 0 °C
실험 절차
A solution of 5-fluoro-2-nitrophenylamine (1 eq) in methylenechloride was treated with trifluoroacetic anhydride (1 eq) and stirred for 10 minutes at 0° C. The mixture was quenched with saturated sodium bicarbonate solution. The organic layer was separated and washed with water, brine, dried and evaporated. To the solution of the trifluoroacetamide (1 eq) in a mixture of toluene, acetonitrile and sodium hydroxide solution (50%) was added benzyltrimethylammonium chloride (1 eq) and dimethyl sulfate (1.2 eq). The biphasic mixture was stirred overnight at room temperature and evaporated. The mixture was taken up in ethyl acetate, washed with water, brine, dried and evaporated. The crude was purified by column chromatography eluting with 1:1 hexanes and ethyl acetate to afford (5-fluoro-2-nitrophenyl)methylamine. MS: MH+=170.
후처리
- customThe mixture was quenched with saturated sodium bicarbonate solution
- customThe organic layer was separated
- washwashed with water, brine
- customdried
- customevaporated
- stirringThe biphasic mixture was stirred overnight at room temperature
- customevaporated
- washwashed with water, brine
- customdried
- customevaporated
- customThe crude was purified by column chromatography
- washeluting with 1:1 hexanes and ethyl acetate
출처 및 근거
- ORD 기록
- ord-827e1e82bae44d098f4df3544470df9d
- 출처 데이터셋
- uspto-grants-2010_06
- 특허 번호
- US07728010B2
연결된 노트
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