HRID1792001

反应详情

EQUATION

反应方程式

HRID 1792001 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A suspension of 7-allyl-8-chloro-1,3-dimethyl-3,7-dihydropurine-2,6-dione (200 mg), cis-2,6-dimethylpiperazine (107 mg), and 1,8-diazabicyclo[5.4.0]undec-7-ene (128 μl) in 1-methyl-2-pyrrolidone (2 ml) was stirred at 150° C. for 50 minutes. The reaction mixture was diluted with ethyl acetate and water, and extracted with ethyl acetate. The aqueous layer was extracted with chloroform, and the combined organic layer was washed with water and dried over magnesium sulfate. The solvent was removed by distillation at reduced pressure to give brown oil. The oil was purified by silica gel column chromatography, and 111 mg of the title compound was obtained from a fraction eluted with methanol-ethyl acetate (1:10).

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. extractionThe aqueous layer was extracted with chloroform
  3. washthe combined organic layer was washed with water
  4. dry with materialdried over magnesium sulfate
  5. customThe solvent was removed by distillation at reduced pressure
  6. customto give brown oil
  7. customThe oil was purified by silica gel column chromatography