HRID1475944

反应详情

EQUATION

反应方程式

HRID 1475944 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of ethyl 7-chloro-2-(4-methoxyphenyl)pyrazolo[1,5-a]pyrimidine-5-carboxylate (767 mg; 2.31 mmol) in methylene chloride (10 mL), methanol (10 mL) and triethylamine (2 mL) was added 10% Pd on carbon (77 mg) and the mixture was cooled to 0° C. The reaction flask was put under vacuum and then hydrogen was introduced using a balloon. A second cycle of vacuum and hydrogen purge was performed and the mixture was stirred at 0° C. for 1.5 h. The mixture was flushed with two cycles of vacuum and nitrogen, diluted with methylene chloride and then filtered through a 0.45 micron filter to remove the catalyst. Concentration afforded the crude product which was triturated in methanol (25 mL) and filtered to afford 485 mg (71%) of the title compound. LCMS m/z 298.1 (M+H)+, ret. time=2.53 min.

WORKUP

后处理

  1. customA second cycle of vacuum and hydrogen purge
  2. customThe mixture was flushed with two cycles of vacuum and nitrogen
  3. additiondiluted with methylene chloride
  4. filtrationfiltered through a 0.45 micron
  5. filtrationfilter
  6. customto remove the catalyst
  7. concentrationConcentration
  8. customafforded the crude product which
  9. customwas triturated in methanol (25 mL)
  10. filtrationfiltered