HRID2064668

反应详情

EQUATION

反应方程式

HRID 2064668 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 1,4,6,7-tetrahydro-pyrazolo[4,3-c]pyridine-3,5-dicarboxylic acid 5-tert-butyl ester 3-ethyl ester [5.105 g, Reference Example 18(d)] and lithium hydroxide monohydrate (0.870 g) in methanol (30 ml) and water (10 ml) was stirred at 55° C. for 2.5 hours. The mixture was acidified with saturated aqueous potassium hydrogen sulfate solution and extracted three times with ethyl acetate. The organic extracts were combined, dried over magnesium sulfate and concentrated in vacuo to yield 1,4,6,7-tetrahydro-pyrazolo[4,3-c]pyridine-3,5-dicarboxylic acid 5-tert-butyl ester (4.442 g) as a pale yellow solid. MS: 268 (M+H)+. HPLC (METHOD G): RT=2.86 minutes.

WORKUP

后处理

  1. extractionextracted three times with ethyl acetate
  2. dry with materialdried over magnesium sulfate
  3. concentrationconcentrated in vacuo