HRID588159

反应详情

EQUATION

反应方程式

HRID 588159 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-(6-chloro-3-methoxy-1-trityl-1H-pyrazolo[4,3-c]pyridin-4-yl)prop-2-yn-1-ol (257 mg, 0.535 mmol) was dissolved in DCM (5 ml) charged with Dess-MartinPeriodinane (341 mg, 0.803 mmol) and allowed to stir for 2 h at rt. The reaction was charged with 5 mL 1N sodium thiosulfate and 5 mL saturated sodium bicarbonate and allowed to stir for 15 minutes. The organic layer was separated and the solvents were concentrated in vacuo. Purification on silica gel, 10-50% EtOAc/hexanes gave 1-(6-chloro-3-methoxy-1-trityl-1H-pyrazolo[4,3-c]pyridin-4-yl)prop-2-yn-1-one (60B, 137 mg, 0.287 mmol, 53.5% yield). MS: [M+H]+ m/z 478.

WORKUP

后处理

  1. stirringto stir for 15 minutes
  2. customThe organic layer was separated
  3. concentrationthe solvents were concentrated in vacuo
  4. customPurification on silica gel, 10-50% EtOAc/hexanes