HRID1525649

反应详情

EQUATION

反应方程式

HRID 1525649 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of 4-(bromomethyl)-N-[(dimethylamino)sulfonyl]-2,5-difluorobenzamide (Preparation 1, 33 mg, 0.092 mmol) in DMSO (1 mL) was added 2-chloro-4-hydroxybenzonitrile (114 mg, 0.092 mmol) and K2CO3 (25 mg, 0.18 mmol). The reaction was stirred at room temperature for 16 hours. The reaction was diluted with DCM (10 mL) and water (20 mL). The organic layer was separated and the aqueous layer extracted with DCM (2×10 mL). The combined organic layers were filtered through a phase separation cartridge and reduced to dryness to give a yellow oil which was purified by reverse phase preparative HPLC to afford the title compound.

WORKUP

后处理

  1. customThe organic layer was separated
  2. extractionthe aqueous layer extracted with DCM (2×10 mL)
  3. filtrationThe combined organic layers were filtered through a phase separation cartridge
  4. customto give a yellow oil which
  5. customwas purified by reverse phase preparative HPLC