HRID1739512

反应详情

EQUATION

反应方程式

HRID 1739512 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 5-ethyl-3-(4-iodobenzyl)-2-trifluoroacetylimino-1,3,4-thiadiazoline (44.1 g) in tetrahydrofuran (300 ml) was added 2N sodium hydroxide (100 ml), followed by stirring at room temperature overnight. Water (300 ml) was added to the reaction mixture, followed by extraction with chloroform (250 ml) twice. The organic layers were washed with a saturated aqueous sodium hydrogencarbonate and were dried over anhydrous magnesium sulfate, followed by removal through distillation. The oily substance so obtained was crystallized from diisopropyl ether, whereby 32.3 g of the title compound was obtained.

WORKUP

后处理

  1. extractionfollowed by extraction with chloroform (250 ml) twice
  2. washThe organic layers were washed with a saturated aqueous sodium hydrogencarbonate
  3. dry with materialwere dried over anhydrous magnesium sulfate
  4. customfollowed by removal through distillation
  5. customThe oily substance so obtained
  6. customwas crystallized from diisopropyl ether