Methylamine → trans 3-bromo-N-methylcinnamamide
反応式
[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]参加物
4
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-003ef67a94ef40c7bce81b5c1eafdba4
- 出典データセット
- uspto-grants-1977_08
- 特許番号
- US04041071
反応ノート
読み込み中…