HRID2380079

反应详情

EQUATION

反应方程式

HRID 2380079 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of Mg(OEt)2 (63 g, 0.55 mole) in toluene, under N2, is treated with dihydro-3-acetyl-(3H)-furanone (141 g, 1.10 mole) at 7°-10° C. over a 15 minute period and stirred at 25°-30° C. for 2 hours. The resultant reaction mixture is treated with a solution of o-nitrobenzoyl chloride (185.7 g, 1.0 mole) in toluene at 25°-35° C. over a 45 minute period, stirred at ambient temperatures for 1.75 hours, treated with 400 mL H2O and heated at 60°-75° until reaction is complete by LC analysis. The resultant reaction mixture is cooled to room temperature and the phases are separated to give the title product as a toluene solution, 875 g, 18% desired product by LC analysis (67% yield). The product solution is used as is in Example 6.

WORKUP

后处理

  1. customThe resultant reaction mixture
  2. stirringstirred at ambient temperatures for 1.75 hours
  3. temperatureheated at 60°-75° until reaction
  4. customThe resultant reaction mixture
  5. customthe phases are separated