HRID2066879

反应详情

EQUATION

反应方程式

HRID 2066879 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

2d (0.12 g), 5-chloro-4-fluoro-2-nitro-phenylamine (0.1 g) and diisopropylethylamine (0.1 mL) were combined in 1.2 mL of DMSO and stirred at 110° C. for 3 days. The mixture was cooled to room temperature, diluted with aqueous NaHCO3 (5 mL) and extracted with EtOAc (5 mL). The organic layer was concentrated under vacuum and purified on column chromatography (eluent: 10 to 50% EtOAc in hexane+0.1% triethylamine) to yield 60a.

WORKUP

后处理

  1. temperatureThe mixture was cooled to room temperature
  2. extractionextracted with EtOAc (5 mL)
  3. concentrationThe organic layer was concentrated under vacuum
  4. custompurified on column chromatography (eluent: 10 to 50% EtOAc in hexane+0.1% triethylamine)