HRID925026
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
2-ethylaniline (12.4 mL, 100 mmol) and NEt3 (15.4 mL, 110 mmol) were added to 100 mL of dichloromethane and cooled to 0° C. Acetyl chloride (7.10 mL 100 mmol) was added dropwise to the cooled aniline solution, affording a peach colored suspension after complete addition. The slurry was warmed to room temperature and heated to reflux overnight. The suspension was taken to dryness and the solid was treated with 200 mL of water. The solid was collected by filtration, washed with 200 mL of diethylether and dried in vacuo, yielding 9.45 g (58%) of white solid. 1H NMR (400 MHz, CDCl3): 7.68 (d, 1H), 7.26-7.11 (m, 4H), 2.59 (q, 2H), 2.18 (s, 3H), 1.22 (t, 3H).
WORKUP
后处理
- customaffording a peach colored suspension
- additionafter complete addition
- temperatureThe slurry was warmed to room temperature
- temperatureheated
- temperatureto reflux overnight
- filtrationThe solid was collected by filtration
- washwashed with 200 mL of diethylether
- customdried in vacuo