HRID601430

反应详情

EQUATION

反应方程式

HRID 601430 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

A solution of 4-benzyloxy-1H-pyridin-2-one (0.60 g, 2.98 mmol) in N,N-dimethylacetamide (10 mL) at 0° C. was treated with sodium hydride (0.086 g, 3.58 mmol) for 30 min, then bromomethyl cyclobutane (0.40 mL, 3.58 mmol) was added and the mixture was stirred at 25° C. for 48 hours. The solution was partitioned between 10% aqueous ammonium chloride solution and dichloromethane, the organic layer was separated, concentrated under reduced pressure and the residue was chromatographed on silica gel, eluting with 1% methanol in dichloromethane to provide the title compound (0.426 g, 53%).

WORKUP

后处理

  1. customThe solution was partitioned between 10% aqueous ammonium chloride solution and dichloromethane
  2. customthe organic layer was separated
  3. concentrationconcentrated under reduced pressure
  4. customthe residue was chromatographed on silica gel
  5. washeluting with 1% methanol in dichloromethane