HRID1746026

反应详情

EQUATION

反应方程式

HRID 1746026 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A well-stirred solution of 2′,3′-Dinitro-3,4,4′,5-tetramethoxy-(Z)-stilbene (0.422 g, 1.08 mmol) in a mixture of acetone-water (2:1) was heated to 50° C. Then sodium thiosulfate (1.88 g, 10.81 mmol, 10.0 equiv) was added and the reaction mixture was heated to reflux for 6 hours. The reaction was cooled to room temperature and water was added. The organic layer was separated and the aqueous layer was extracted with ethyl acetate (4×25 mL). The combined organic layer were washed with brine, dried over Na2SO4 and concentrated in vacuo. The mixture was then subjected to preparative TLC to give the 2′,3′-Diamino-3,4,4′,5-tetramethoxy-(Z)-stilbene.

WORKUP

后处理

  1. temperaturethe reaction mixture was heated
  2. temperatureto reflux for 6 hours
  3. temperatureThe reaction was cooled to room temperature
  4. customThe organic layer was separated
  5. extractionthe aqueous layer was extracted with ethyl acetate (4×25 mL)
  6. washThe combined organic layer were washed with brine
  7. dry with materialdried over Na2SO4
  8. concentrationconcentrated in vacuo