HRID1613184

反应详情

EQUATION

反应方程式

HRID 1613184 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-amino-2-methylpropanol (89.1 g), benzhydrol (190 g) and para-toluenesulphonic acid monohydrate (200 g) in toluene (1200 ml) was heated under reflux in a Dean-Stark apparatus for four hours and evaporated. The residue was partitioned between ether and water and the organic layer was washed with water and extracted into 10% aqueous citric acid. The acidic extract was washed with ether, basified with solid sodium carbonate and extracted into ether. The organic extract was washed with water, dried over sodium sulphate and evaporated to give the title compound as a pale yellow oil (177 g, 69%) which was characterised by its 1H-n.m.r. spectrum.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux in a Dean-Stark apparatus for four hours
  3. customevaporated
  4. customThe residue was partitioned between ether and water
  5. washthe organic layer was washed with water
  6. extractionextracted into 10% aqueous citric acid
  7. extractionThe acidic extract
  8. washwas washed with ether
  9. extractionextracted into ether
  10. extractionThe organic extract
  11. washwas washed with water
  12. dry with materialdried over sodium sulphate
  13. customevaporated