HRID732234

反应详情

EQUATION

反应方程式

HRID 732234 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

To a mixture of 3.0 g of pteroic acid and 5.35 mL of triethylamine (TEA), 6.24 g of CDI as dissolved in 50 mL of DMSO was added and reacted at room temperature for 3.5 hours. To the reaction solution 2-(trimethylsilyl)ethanol (9.63 mL) was added, followed by further 5 hours' reaction at room temperature. The reaction solution was added dropwise into water (10 mL)-acetic acid (0.32 mL) and dimethyl ether (6.4 mL), vigorously stirred for a few minutes, and recovered as solid by suction filtration. The solid product was purified by column chromatography (silica gel column: eluent; 10% methanol in chloroform) and dried under reduced pressure to finally give 2.67 g (yield=54.8%) of aimed compound.

WORKUP

后处理

  1. additionwas added
  2. customreacted at room temperature for 3.5 hours
  3. custom' reaction at room temperature
  4. filtrationrecovered as solid by suction filtration
  5. customThe solid product was purified by column chromatography (silica gel column: eluent; 10% methanol in chloroform)