HRID68608

反应详情

EQUATION

反应方程式

HRID 68608 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

To a solution of 5-Formyl-2-methoxyphenylboronic acid (324 mg, 1.8 mmol, 1.5 eq, Frontier Scientific, Inc., Logan, Utah, USA) in dioxane:H2O (2:1; 15 mL) was added 4-bromo-1-fluoro-2-(methylsulfonyl)benzene (300 mg, 1.2 mmol, 1.0 eq., Apollo Scientific Ltd., Stockport, Cheshire, UK), K2CO3 (496 mg, 3.6 mmol, 2 eq.) and Pd(PPh3)4 (30 mg). The mixture was stirred under nitrogen at 140° C. in a microwave for 40 min. Solvent was evaporated and the residue was dissolved in DCM and washed with water. The DCM layer was dried and evaporated. Purification via column chromatography (eluent: PE:EA=3:1) yielded 400 mg (72%) of 3-(4-fluoro-3-(methylsulfonyl)phenyl)-4-methoxybenzaldehyde (27).

WORKUP

后处理

  1. customSolvent was evaporated
  2. dissolutionthe residue was dissolved in DCM
  3. washwashed with water
  4. dry with materialThe DCM layer was dried
  5. customevaporated
  6. customPurification via column chromatography (eluent: PE:EA=3:1)