Methylamine → trans 3-bromo-N-methylcinnamamide
반응식
[Br:1][C:2]1[CH:3]=[C:4]([CH:10]=[CH:11][CH:12]=1)/[CH:5]=[CH:6]/[C:7](Cl)=[O:8].[CH3:13][NH2:14]>C1C=CC=CC=1>[Br:1][C:2]1[CH:3]=[C:4]([CH:10]=[CH:11][CH:12]=1)/[CH:5]=[CH:6]/[C:7]([NH:14][CH3:13])=[O:8]참가 물질
4
실험 절차
A solution of trans 3-bromocinnamoyl chloride (5 g) in dry benzene (100 ml) was added with stirring to an ethereal (200 ml) solution of methylamine (3 g). After the addition was complete, a slow stream of methylamine gas was bubbled through the reaction mixture at room temperature for 1 hour. Solvent and excess amine were removed under reduced pressure. The crude product was triturated with water, filtered, and recrystallized from ethanol-water to give trans 3-bromo-N-methylcinnamamide, m.p. 147°-147.5° C. NMR, IR, and elemental analysis were consistent with this structure.
후처리
- additionAfter the addition
- customa slow stream of methylamine gas was bubbled through the reaction mixture at room temperature for 1 hour
- customSolvent and excess amine were removed under reduced pressure
- customThe crude product was triturated with water
- filtrationfiltered
- customrecrystallized from ethanol-water
출처 및 근거
- ORD 기록
- ord-003ef67a94ef40c7bce81b5c1eafdba4
- 출처 데이터셋
- uspto-grants-1977_08
- 특허 번호
- US04041071
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