HRID2254879

反应详情

EQUATION

反应方程式

HRID 2254879 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1.70g (0.005 mole) of 3-(3,5-di-tertiary-butyl-4-hydroxyanilino)benzoic acid (prepared in Example 13) and 50 ml of hot isopropyl alcohol was filtered to remove a small amount of insoluble material. The resulting solution was deoxygenated with a stream of nitrogen gas. Uner a nitrogen atmosphere, a solution of 0.44g (0.005 mole) of morpholine in 1.5 ml of isopropyl alcohol was added with rapid stirring. Evaporation provided a solid which was recrystallized from a mixture of isopropyl alcohol and isopropyl ether to give solid morpholinium-3-(3,5-di-tertiary-butyl-4-hydroxyanilino)benzoate, m.p. 147°-150° C. Analysis: Calculated for C21H27NOC4H9NO: %C, 70.1; %H, 8.5; %N, 6.5; Found: %C, 69.8; %H, 8.5; %N, 6.4.

WORKUP

后处理

  1. filtrationwas filtered
  2. customto remove a small amount of insoluble material
  3. customThe resulting solution was deoxygenated with a stream of nitrogen gas
  4. customEvaporation
  5. customprovided a solid which
  6. customwas recrystallized from a mixture of isopropyl alcohol and isopropyl ether