HRID1900747

反应详情

EQUATION

反应方程式

HRID 1900747 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-bromomethyl-5-methyl-2,3,6,7-tetrahydrofuro-[2,3-f]quinoline-7-one (2.942 g) in dimethylformamide (120 ml) was combined with aqueous 15% sodium thiomethoxide (9.4 ml), and stirred at room temperature for 1 hour. The solvent was distilled off under reduced pressure. Water was added to the residue, and extracted with chloroform. The chloroform extract was washed with diluted hydrochloric acid, diluted caustic soda and water in this order, and dried. The resultant material was crystallized from tetrahydrofuran to obtain 2.355 g of the title compound as colorless prisms (mp. 203°-206° C.) (yield: 90.1%).

WORKUP

后处理

  1. distillationThe solvent was distilled off under reduced pressure
  2. additionWater was added to the residue
  3. extractionextracted with chloroform
  4. extractionThe chloroform extract
  5. washwas washed with diluted hydrochloric acid, diluted caustic soda and water in this order
  6. customdried
  7. customThe resultant material was crystallized from tetrahydrofuran