HRID657378

反应详情

EQUATION

反应方程式

HRID 657378 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of ethyl 3-({[1,6-diethyl-4-(tetrahydro-2H-pyran-4-ylamino)-1H-pyrazolo[3,4-b]pyridin-5-yl]methyl}amino)-3-oxopropanoate (130 mg, 0.30 mmol), LiOH (63 mg, 1.5 mmol), water (1 mL) and ethanol (2 mL) was stirred at room temperature overnight. The aqueous layer was acidified with 2 N HCl to PH<1. Brine (30 mL) was added to the solution. The aqueous layer was extracted with a mixture of DCM:IPA (4:1) twice. The organic layer was dried over sodium sulfate, filtered and then concentrated under vacuum to give 3-({[1,6-diethyl-4-(tetrahydro-2H-pyran-4-ylamino)-1H-pyrazolo[3,4-b]pyridin-5-yl]methyl}amino)-3-oxopropanoic acid (88 mg, 75%). LC-MS m/z 390 (M+H)+.

WORKUP

后处理

  1. extractionThe aqueous layer was extracted with a mixture of DCM:IPA (4:1) twice
  2. dry with materialThe organic layer was dried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated under vacuum