HRID357484

反应详情

EQUATION

反应方程式

HRID 357484 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4.38 g (25 mmol) of 2-chloro-4,6-dimethoxypyrimidine, 2.31 g (26.2 mmol) of 3-hydroxy-2-oxobutane and 0.66 g (6.3 mmol) of sodium methanesulfinate were heated in the presence of 5.17 g (37.5 mmol) of potassium carbonate in 25 ml of N,N-dimethylformamide to 120° C. with stirring. After 3 hours, the solvent was removed in a rotary evaporator at 70° C./20 mbar. The residue was purified by chromatography on a silica gel column (eluent hexane/ethyl acetate 4:1). The title product was obtained from the product fraction in the form of a pale yellowish oil in a yield of 4.58 g (80.4 percent of theory) (GC content 99 percent). Other data concerning the title compound was:

WORKUP

后处理

  1. customthe solvent was removed in a rotary evaporator at 70° C./20 mbar
  2. customThe residue was purified by chromatography on a silica gel column (eluent hexane/ethyl acetate 4:1)