HRID1888367

反应详情

EQUATION

反应方程式

HRID 1888367 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

The mixture of 5-amino-2-bromobenzoic acid methyl ester (14.27 g, 62.0 mmol) and CuCN (6.11 g, 68.2 mmol) in DMF (130 ml) was heated at 150° C. for 1 h 10 min under nitrogen atmosphere. The mixture was cooled to 70° C. and poured into the mixture of water (250 ml) and 12.5% NH3 (500 ml). The product was extracted into ethyl acetate (3×250 ml). The organic phase was washed several times with 12.5% NH3 and water, dried over Na2SO4 and concentrated under vacuum.

WORKUP

后处理

  1. temperatureThe mixture was cooled to 70° C.
  2. extractionThe product was extracted into ethyl acetate (3×250 ml)
  3. washThe organic phase was washed several times with 12.5% NH3 and water
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated under vacuum