HRID380684

反应详情

EQUATION

反应方程式

HRID 380684 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-chloro-3-fluorobenzoic acid (0.098 g) and carbonyldiimidazole (0.091 g), in N,N-dimethylformamide (3.0 ml) was stirred for 2.5 hours at room temperature. 1-Adamantanemethylamine (0.1 ml) was then added and stirring continued overnight. The reaction mixture was partitioned between ethyl acetate and 2N hydrochloric acid and the organic layer was separated, washed with 10% aqueous sodium hydroxide, water and brine and then dried over sodium sulphate (Na2SO4). The organic layer was subsequently concentrated under reduced pressure to yield the tire compound as a white solid (0.138 g).

WORKUP

后处理

  1. customThe reaction mixture was partitioned between ethyl acetate and 2N hydrochloric acid
  2. customthe organic layer was separated
  3. washwashed with 10% aqueous sodium hydroxide, water and brine
  4. dry with materialdried over sodium sulphate (Na2SO4)
  5. concentrationThe organic layer was subsequently concentrated under reduced pressure