HRID1952357

反应详情

EQUATION

反应方程式

HRID 1952357 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution methyl [1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazolo[3,4-b]pyridin-3-yl]acetate (128 mg, 0.465 mmol) at 0° C. was added 2M LAH in THF (232 ul, 0.465 mmol) and stirred at 0° C. for 30 minutes. After this time, the reaction mixture was sequentially treated with water (18 ul) and 1.0N NaOH (54 ul) and stirred at 25° C. for 30 minutes. After this time, the mixture was filtered through celite and rinsing with THF. The filtrates were combined and the solvent evaporated in vacuo. The residue was purified by chromatography using RediSep column (12 g) and eluting with a gradient of 0-10% MeOH/CH2Cl2 to give the title compound. LRMS (M+1): 164.0.

WORKUP

后处理

  1. stirringstirred at 25° C. for 30 minutes
  2. filtrationAfter this time, the mixture was filtered through celite
  3. washrinsing with THF
  4. customthe solvent evaporated in vacuo
  5. customThe residue was purified by chromatography
  6. washeluting with a gradient of 0-10% MeOH/CH2Cl2