HRID1973393

反应详情

EQUATION

反应方程式

HRID 1973393 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

One-half (by volume) of the resultant solution of 4-(tert-butyl)benzenesulfenyl chloride was added to a solution of 10.9 g of carbofuran in 30 ml of pyridine. The mixture was allowed to stand overnight, then poured into water. The water-insoluble material was washed several times with water, then dissolved in ether. The ether solution was washed with water and dried. Removal of the ether under reduced pressure gave a solid which on recrystallization from hexane-ether gave 7.5 g of solid, m.p. 120°-3°. Four recrystallizations from hexane gave 2,3-dihydro-2,2-dimethyl-7-benzofuranyl [4-(tert-butyl)phenylthio] (methyl)carbamate, m.p. 122°-123°. The n.m.r. spectrum was consistent with the assigned structure.

WORKUP

后处理

  1. washThe water-insoluble material was washed several times with water
  2. dissolutiondissolved in ether
  3. washThe ether solution was washed with water
  4. customdried
  5. customRemoval of the ether under reduced pressure
  6. customgave a solid which
  7. customon recrystallization from hexane-ether