HRID889047

反应详情

EQUATION

反应方程式

HRID 889047 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
95 °C

PROCEDURE

实验过程

A mixture of 1,3-dipropyl-8-(1H-pyrazol-4-yl)-7-(2-trimethylsilanyl-ethoxymethyl)-3,7-dihydro-purine-2,6-dione (0.200 g, 0.462 mmol), 4-(2-Bromo-acetyl)-1-(3-trifluoromethyl-phenyl)-pyrrolidin-2-one (0.240 g, 0.693 mmol), Cs2CO3 (0.30 g, 0.924 mmol) and acetonitrile (2 ml) were heated at 90-100° C. in a sealed tube for 6 hrs. Reaction mixture was cooled to 20-25° C. and filtered off. The organic volatiles were evaporated. The crude product was purified by preparative TLC to obtain pure 8-(1-{2-oxo-2-[5-oxo-1-(3-trifluoromethyl-phenyl)-pyrrolidin-3-yl]-ethyl}-1H-pyrazol-4-yl)-1,3-dipropyl-7-(2-trimethylsilanyl-ethoxymethyl)-3,7-dihydro-purine-2,6-dione (0.090 g, 28%) as a brown mass.

WORKUP

后处理

  1. customReaction mixture
  2. temperaturewas cooled to 20-25° C.
  3. filtrationfiltered off
  4. customThe organic volatiles were evaporated
  5. customThe crude product was purified by preparative TLC