HRID2246629

反应详情

EQUATION

反应方程式

HRID 2246629 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Sodium hydride (60% in mineral oil, 12 mg) was added to N-cyclopropyl-3-fluoro-5-(1H-indazol-5-yl)-4-methylbenzamide (Intermediate 3, 45 mg) in DMF (5 ml) and the mixture was stirred at room temperature for 1 h. 2-(Bromomethyl)tetrahydro-2H-pyran (20.5 μl) was added and stirring continued for 18 h. The mixture was diluted with chloroform/ethyl acetate (1:1, 5 ml) and washed with water (2×5 ml). The organic phase was concentrated under vacuum and the residue was purified by preparative HPLC to give the title compound as a colourless glass (23 mg).

WORKUP

后处理

  1. stirringstirring
  2. waitcontinued for 18 h
  3. washwashed with water (2×5 ml)
  4. concentrationThe organic phase was concentrated under vacuum
  5. customthe residue was purified by preparative HPLC