HRID1583033

反应详情

EQUATION

反应方程式

HRID 1583033 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2,4-Difluorobenzyl bromide (0.77 mL, 6 mmol, 1 eq) was added dropwise to a stirred solution of 5-formylsalicylic acid (1 g, 6 mmol, 1 eq) and cesium carbonate (5.87 g, 18 mmol, 3 eq) in N,N-dimethylformamide (30 mL). The reaction mixture was diluted with ethyl acetate (50 mL) and the organic solution washed with water (50 mL), saturated aqueous sodium bicarbonate (2×50 mL) and brine (50 mL), then dried over sodium sulfate and evaporated in vacuo to give the product as a white powder (1.2 g, 50%). 1H NMR (CDCl3) δ9.91 (s, 1H, O═C—H), 5.37 (s, 2H, CH2Ar), 5.25 (s, 2H, CH2Ar).

WORKUP

后处理

  1. washthe organic solution washed with water (50 mL), saturated aqueous sodium bicarbonate (2×50 mL) and brine (50 mL)
  2. dry with materialdried over sodium sulfate
  3. customevaporated in vacuo