HRID233917

反应详情

EQUATION

反应方程式

HRID 233917 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 of [4-(6-fluoro-1H-indazol-3-yl)-1-piperidinyl]-acetonitrile (6.1 g, 23.6 mmol) in dry THF (235 ml) was added (dropwise) lithium aluminum hydride (LAH) (28.4 mmol, 1.0M in THF) at room temperature, under nitrogen. Upon complete addition, the reaction mixture was warmed to reflux for 3 hours. After cooling to 0° C. in an ice bath, the reaction was carefully quenched with water (4.0 ml). The solids were removed via filtration and washed with THF. The combined filtrates were concentrated to give 5.6 g of the desired product. This material was suspended in DCM and filtered to give the product as an off-white solid, m.p. 125°-128° C.

WORKUP

后处理

  1. additionUpon complete addition
  2. temperaturethe reaction mixture was warmed
  3. temperatureto reflux for 3 hours
  4. customthe reaction was carefully quenched with water (4.0 ml)
  5. customThe solids were removed via filtration
  6. washwashed with THF
  7. concentrationThe combined filtrates were concentrated