HRID1048084

反应详情

EQUATION

反应方程式

HRID 1048084 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

2-(2-chloro-4-fluorophenyl)acetamide (400 mg, 2.13 mmol) was diluted with THF (2 mL), placed under nitrogen and cooled to 0° C. LAH (4264 μL, 4.26 mmol) was added dropwise and the reaction was refluxed for 3 hours. The reaction was cooled to 0° C. and quenched with 160 μL of water, 160 μL of 15% NaOH, and 530 μL of water. After stirring for 30 minutes the reaction was filtered and concentrated. The material was purified using a biotage 25 column eluting with 2% NH4OH/10% methanol/DCM to yield 2-(2-chloro-4-fluorophenyl)ethanamine (60 mg, 0.346 mmol, 16.2% yield).

WORKUP

后处理

  1. temperaturethe reaction was refluxed for 3 hours
  2. temperatureThe reaction was cooled to 0° C.
  3. customquenched with 160 μL of water, 160 μL of 15% NaOH, and 530 μL of water
  4. filtrationwas filtered
  5. concentrationconcentrated
  6. customThe material was purified
  7. washeluting with 2% NH4OH/10% methanol/DCM