HRID1524289

反应详情

EQUATION

反应方程式

HRID 1524289 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

Split a solution of trans-3-(3-bromo-phenyl)-4-(3-cyano-phenylcarbamoyl)-pyrrolidine-1-carboxylic acid tert-butyl ester (0.53 g, 1.13 mmol) in a 1:1 mixture of MeOH/THF (10 mL) into three microwave pressure tubes. Add to each tube molybedinum hexacarbonyl (0.06 g, 0.23 mmol) followed by N,N-diisoproylethyl amine (0.15 mL, 0.80 mmol) and Herrmann's palladacycle (0.16 g, 0.17 mmol). Heat each mixture in a microwave reactor at 150° C. for 15 minutes then cool to room temperature. Combine the mixtures, dilute with EtOAc and load onto silica gel. Purify the residue by flash silica gel chromatography to provide 0.20 g of trans-3-(3-cyano-phenylcarbamoyl)-4-(3-methoxycarbonyl-phenyl)-pyrrolidine-1-carboxylic acid tert-butyl ester as a foam.

WORKUP

后处理

  1. additionAdd to each tube molybedinum hexacarbonyl (0.06 g, 0.23 mmol)
  2. temperaturethen cool to room temperature
  3. customPurify the residue by flash silica gel chromatography