HRID2251863

反应详情

EQUATION

反应方程式

HRID 2251863 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

The mixture of 3-bromomethyl-7-nitro-3H-isobenzofuran-1-one (0.50 g, 1.84 mmol, Step E) and 4-tert-butylaniline (1.20 mL, 7.36 mmol) in 20 mL of THF was slowly warmed to RT from 0° C., then heated to reflux for 24 h. After cooling to RT, the mixture was diluted with H2O, and extracted with EtOAc. The combined organic portions were washed with brine, dried over MgSO4, filtered, condensed, and the titled compound was obtained as a light yellowish solid after column chromatography (10 to 35% of EtOAc in hexanes).

WORKUP

后处理

  1. temperatureheated
  2. temperatureto reflux for 24 h
  3. temperatureAfter cooling to RT
  4. extractionextracted with EtOAc
  5. washThe combined organic portions were washed with brine
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. customcondensed