HRID72987

反应详情

EQUATION

反应方程式

HRID 72987 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To 3-fluoro-4-methylsulfonyl-benzoic acid (490 mg, 2.25 mmol), sodium hydride (270 mg, 6.74 mmol), methanol (1.55 g, 2.0 mL, 48.3 mmol) was added DMF (5 mL) and reaction mixture was heated at 100° C. for 1 hour. The reaction mixture was cooled and diluted with EtOAc and acidified using 1 M HCl solution. The organic layer was separated, washed with saturated aqueous brine solution (3×), dried over sodium sulfate and concentrated in vacuo to give 3-methoxy-4-methylsulfonyl-benzoic acid (496 mg, 95%). ESI-MS m/z calc. 230.0. Found 231.3 (M+1)+; Retention time: 0.49 minutes (3 min run).

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled
  2. customThe organic layer was separated
  3. washwashed with saturated aqueous brine solution (3×)
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated in vacuo