HRID1773770

反应详情

EQUATION

反应方程式

HRID 1773770 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 1M solution of lithium aluminum hydride in THF (6.5 mL, 6.5 mmol) was added dropwise to a stirred solution of 4,5,6,7-tetrahydro-4-oxo-5-(phenylmethyl)-pyrazolo[1,5-a]pyrazine-2-carboxylic acid ethyl ester (0.81 g, 2.7 mmol) in THF (16 mL) under N2 at 0° C. The reaction mixture was stirred at room temperature for 30 minutes, quenched with MeOH and the solvents evaporated in vacuo. The crude product was purified by flash column chromatography (silica; 7 M solution of ammonia in methanol in DCM 0/100 to 10/90). The desired fractions were collected and the solvents evaporated in vacuo to yield 4,5,6,7-tetrahydro-5-(phenylmethyl)-pyrazolo[1,5-a]pyrazine-2-methanol (0.67 g, 100% yield) as a colorless oil. C14H17N3O LCMS: Rt 1.25, m/z 244 [M+H]+ (see LCMS Method 1).

WORKUP

后处理

  1. customquenched with MeOH
  2. customthe solvents evaporated in vacuo
  3. customThe crude product was purified by flash column chromatography (silica; 7 M solution of ammonia in methanol in DCM 0/100 to 10/90)
  4. customThe desired fractions were collected
  5. customthe solvents evaporated in vacuo