HRID2364766

反应详情

EQUATION

反应方程式

HRID 2364766 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The crude compound (7S)-2-chloro-8-isopropyl-7-ethyl-5,7-dihydropteridin-6-one 43c (7.17 g, 28.21 mmol), methyl p-toluenesulfonate (5.77 g, 31.03 mmol) and potassium carbonate (11.70 g, 84.60 mmol) were dissolved in 40 mL of acetone. The reaction solution was stirred for 12 hours and the precipite was filtered. The filter cake was washed with dichloromethane (100 mL). The filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography with elution system B to obtain (7S)-2-chloro-8-isopropyl-7-ethyl-5-methyl-7H-pteridin-6-one 43d (6.14 g, yield: 81.0%) as a white solid.

WORKUP

后处理

  1. filtrationthe precipite was filtered
  2. washThe filter cake was washed with dichloromethane (100 mL)
  3. concentrationThe filtrate was concentrated under reduced pressure
  4. customThe resulting residue was purified by silica gel column chromatography with elution system B