HRID1051514

反应详情

EQUATION

反应方程式

HRID 1051514 的结构方程式

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of 3-bromobenzene-1,2-diamine (2 g, 10.7 mmol) in HCOOH was stirred at 100° C. for 1 h. The mixture was cooled and concentrated in vacuo and diluted with ethyl acetate and aq. NaHCO3. The mixture was extracted further with ethyl acetate and the combined organic layers dried and concentrated to give the crude product which was purified by column chromatography to obtain the desired product (1.65 g, Yield 80%). LCMS (m/z): 197.0 (M+1).

WORKUP

后处理

  1. temperatureThe mixture was cooled
  2. concentrationconcentrated in vacuo
  3. additiondiluted with ethyl acetate and aq. NaHCO3
  4. extractionThe mixture was extracted further with ethyl acetate
  5. customthe combined organic layers dried
  6. concentrationconcentrated
  7. customto give the crude product which
  8. customwas purified by column chromatography