HRID1973394

反应详情

EQUATION

反应方程式

HRID 1973394 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 8.75 g of 4-methylbenzenesulfenyl chloride in 25 ml of pyridine was added to a solution of 10.9 g of carbofuran in 25 ml of pyridine. A precipitate formed immediately. The reaction mixture was processed as described in Example I to give a residue which could not be distilled even at 0.005 mm. Passage through a falling film still at 140° at 0.01 mm, then at 168° at 0.01 mm gave a liquid which crystallized on standing to a solid, m.p. 62°. Recrystallization several times from petroleum ether gave 2,3-dihydro-2,2-dimethyl-7-benzofuranyl (methyl)(4-methylphenylthio)carbamate, m.p. 65°.

WORKUP

后处理

  1. customA precipitate formed immediately
  2. customto give a residue which could not
  3. distillationbe distilled even at 0.005 mm
  4. customPassage through a falling film still at 140° at 0.01 mm, then at 168° at 0.01 mm gave a liquid which
  5. customcrystallized
  6. customRecrystallization several times from petroleum ether