HRID647226

反应详情

EQUATION

反应方程式

HRID 647226 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred solution of 6-amino-2,5-dimethylbenzoxazole (14.8 g, 0.1 mol) in 100 ml of pyridine and 500 ml of dichloromethane was added N,N-dioctadecyl-3-chlorosulfonylbenzamide (72.4 g, 0.1 mol). The mixture was stirred overnight and then washed with water, 10 percent aqueous hydrochloric acid and again with water. To the organic layer was added 10 ml of hydrochloric acid, 300 ml of water and 1000 ml of THF. The mixture was stirred overnight and the precipitate collected, washed with acetonitrile and nearly dried. The damp filter cake was placed in 2 liters of THF and 50 ml of concentrated hydrochloric acid and refluxed 2 hours. The mixture was concentrated to an oil and triturated with one liter of acetonitrile to yield 77.5 g (90 percent) of the product.

WORKUP

后处理

  1. washwashed with water, 10 percent aqueous hydrochloric acid and again with water
  2. additionTo the organic layer was added 10 ml of hydrochloric acid, 300 ml of water and 1000 ml of THF
  3. stirringThe mixture was stirred overnight
  4. customthe precipitate collected
  5. washwashed with acetonitrile
  6. customnearly dried
  7. temperature50 ml of concentrated hydrochloric acid and refluxed 2 hours
  8. concentrationThe mixture was concentrated to an oil
  9. customtriturated with one liter of acetonitrile