HRID1716605

反应详情

EQUATION

反应方程式

HRID 1716605 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
180 °C

PROCEDURE

实验过程

A mixture of 1-chloro-5-fluoro-4-methyl-2-nitro-benzene (2 g, 10.55 mmol), 4-amino-piperidine-1-carboxylic acid tert-butyl ester (2.32 g, 11.58 mmol), and iPr2NEt (3.8 mL) was heated for 2 hours at 180° C. by microwave heating. After cooling, the reaction mixture was diluted with CH2Cl2 and then filtered. The volatiles were removed under reduced pressure and the residue was purified by flash chromatography (25% ethyl acetate in hexanes) to afford 4-(5-fluoro-4-methyl-2-nitro-phenylamino)piperidine-1-carboxylic acid tert-butyl ester (0.68 g, 18%) as a brown solid.

WORKUP

后处理

  1. temperatureheating
  2. temperatureAfter cooling
  3. filtrationfiltered
  4. customThe volatiles were removed under reduced pressure
  5. customthe residue was purified by flash chromatography (25% ethyl acetate in hexanes)