HRID1021461

反应详情

EQUATION

反应方程式

HRID 1021461 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)-4-chloro-2-methoxy-1-(2-nitrovinyl)benzene (245 mg, 1.15 mmol) was diluted with THF (1 mL), placed under nitrogen and cooled to 0° C. LAH (4588 μL, 4.59 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 174 μL of water, 174 μL of 15% NaOH and 522 μL water. After stirring for 1 hour, ethyl acetate and MgSO4 was added. The reaction mixture was filtered and concentrated to yield 2-(4-chloro-2-methoxyphenyl)ethanamine (160 mg, 0.862 mmol, 75.1% yield).

WORKUP

后处理

  1. temperaturewarming to ambient temperature
  2. temperatureThe reaction was cooled to 0° C.
  3. customquenched with 174 μL of water, 174 μL of 15% NaOH and 522 μL water
  4. stirringAfter stirring for 1 hour
  5. additionethyl acetate and MgSO4 was added
  6. filtrationThe reaction mixture was filtered
  7. concentrationconcentrated