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 one 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 one 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-ae489c040dda47288ee03333979fc070
- 出典データセット
- uspto-grants-1978_05
- 特許番号
- US04091112
反応ノート
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