HRID1730379

反应详情

EQUATION

反应方程式

HRID 1730379 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a cold (5° C.) solution of 3 moles of diethanolamine in tetrahydrofuran was added dropwise a solution of 3,5-di-t-butyl-4-hydroxybenzoyl chloride in benzene. The reaction mixture was stirred for about 1 hour, washed with water, separating the benzene layer from the aqueous layer. The benzene solution was evaporated to yieldan oil, which, after crystallization with aqueous ethanol, yielded a white solid. Small amounts of by-product compounds of Examples 1 and 3 were removed by fractional crystallization to yield N-hydroxyethyl-N-(3',5'-di-t-butyl-4'-hydroxybenzoyloxyethyl)-3,5-di-t-butyl-4-hydroxybenzamide; melting point 174°-178° C. When testedby the procedure of Example 2, the sample containing this compound lasted 1,200 hours, about 2.2 times as long as the control.

WORKUP

后处理

  1. washwashed with water
  2. customseparating the benzene layer from the aqueous layer
  3. customThe benzene solution was evaporated
  4. customafter crystallization with aqueous ethanol
  5. customyielded a white solid
  6. customSmall amounts of by-product compounds of Examples 1 and 3 were removed by fractional crystallization