HRID573079

反应详情

EQUATION

反应方程式

HRID 573079 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

Tert-butyl 4-aminopiperidine-1-carboxylate (8.63 g) was dissolved in 1,4-dioxane (250 mL), and 4-chloro-3-nitrobenzenesulfonamide (6.00 g) was added followed by triethylamine (10.60 mL). The solution was heated at 90° C. for 20 hours and then cooled. The solvent was removed under vacuum, and the material was purified by flash column chromatography on silica gel using 50% ethyl acetate in hexanes, increasing to 100% ethyl acetate and increasing further to 20% methanol in dichloromethane.

WORKUP

后处理

  1. temperaturecooled
  2. customThe solvent was removed under vacuum
  3. customthe material was purified by flash column chromatography on silica gel using 50% ethyl acetate in hexanes
  4. temperatureincreasing to 100% ethyl acetate
  5. temperatureincreasing further to 20% methanol in dichloromethane