HRID1021458

反应详情

EQUATION

反应方程式

HRID 1021458 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

(E)-2-chloro-1-(2-nitrovinyl)-4-(trifluoromethyl)benzene (160 mg, 0.636 mmol) was diluted with THF (1 mL), placed under nitrogen and cooled to 0° C. LAH (2544 μL, 2.54 mmol) was added dropwise and the reaction was stirred for 5 hours warming to ambient temperature. The reaction was cooled to 0° C. and quenched with 100 μL of water, 100 μL of 15% NaOH and 300 μL water. After stirring for 1 hour, ethyl acetate and MgSO4 was added. The reaction mixture was filtered and concentrated to yield 2-(2-chloro-4-(trifluoromethyl)phenyl)ethanamine (60 mg, 0.268 mmol, 42.2% yield).

WORKUP

后处理

  1. temperaturewarming to ambient temperature
  2. temperatureThe reaction was cooled to 0° C.
  3. customquenched with 100 μL of water, 100 μL of 15% NaOH and 300 μL water
  4. stirringAfter stirring for 1 hour
  5. additionethyl acetate and MgSO4 was added
  6. filtrationThe reaction mixture was filtered
  7. concentrationconcentrated