HRID18109

反应详情

EQUATION

反应方程式

HRID 18109 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To the compound of Example 194 (0.36 g) in dimethylformamide was added lithium chloride (0.096 g), tetramethyl tin (0.126 ml) and dichlorobis(triphenylphosphine) palladium (0) (0.035 g) and the resulting mixture heated at 100° C. under argon for 18 h. The reaction was then evaporated, diluted with dichloromethane, filtered and the filtrate washed with water, dried and evaporated. Chromatography of the residue on silica gel, eluting with methanol-dichloromethane mixtures, afforded the title product (0.2 g) as a yellow amorphous solid. Mass Spectrum (API+): Found 412 (MH+). C21H22FN5OS requires 411.

WORKUP

后处理

  1. customThe reaction was then evaporated
  2. additiondiluted with dichloromethane
  3. filtrationfiltered
  4. washthe filtrate washed with water
  5. customdried
  6. customevaporated
  7. washChromatography of the residue on silica gel, eluting with methanol-dichloromethane mixtures