HRID644214

反应详情

EQUATION

反应方程式

HRID 644214 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4-Hydroxycyclohexanone-1,1-ethylene ketal (0.63 g, 4 mmol), 2-[4-isopropyl-2-hydroxybenzoylamino]-N-(5-chloropyridin-2-yl)benzamide (1.64 g, 4 mmol), triphenyl-phosphine (1.05 g, 4 mmol), and dry DMF (2 mL) were sonicated for 5 min at room temperature. DIAD (0.8 mL, 4 mmol) was added and sonication was continued for 1 h. Ether (40 mL) was added and the solution was chilled overnight in the freezer to crystallize triphenylphosphine oxide. The crystals were filtered, washed with a little ether, and the combined filtrates were evaporated to dryness to give a yellow oil.

WORKUP

后处理

  1. customsonication
  2. temperaturethe solution was chilled overnight in the freezer
  3. customto crystallize triphenylphosphine oxide
  4. filtrationThe crystals were filtered
  5. washwashed with a little ether
  6. customthe combined filtrates were evaporated to dryness
  7. customto give a yellow oil