反応 #63498

反応方程式

β-(3,4-dimethoxyphenyl)ethylamine

triethylamine

acetyl chloride

→

N-acetyl-3,4-dimethoxyphenethylamine

収率 91.0%

溶媒

CHCl3

反応条件

後処理

1. 1
   洗浄The mixture was washed with 3×500 ml H2O
2. 2
   乾燥dried over MgSO4
3. 3
   その他evaporated to a solid
4. 4
   workup.DISSOLUTIONThe solid was dissolved in 500 ml hot CCl4
5. 5
   workup.ADDITION300 ml cyclohexane added
6. 6
   温度to cool slowly
7. 7
   ろ過The crystallized solid was collected by filtration
8. 8
   その他dried

実験手順

To a stirred solution of β-(3,4-dimethoxyphenyl)ethylamine (100 g, 0.552 m) and triethylamine (66.6 g, 0.66 m) in CHCl3 (1 liter) was added acetyl chloride (47.1 g, 0.60 mole) dropwise over a period of 30 min. and the mixture stirred overnight. The mixture was washed with 3×500 ml H2O, dried over MgSO4 and evaporated to a solid. The solid was dissolved in 500 ml hot CCl4, 300 ml cyclohexane added and allowed to cool slowly. The crystallized solid was collected by filtration and dried to afford N-acetyl-3,4-dimethoxyphenethylamine as a white solid, 112.1 g (91% yield). m.p. 99°-100°.

出典