HRID1613192

反应详情

EQUATION

反应方程式

HRID 1613192 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-methyl-2-methylaminopropanol (1.5 g), 3,4-methylenedioxybenzyl chloride (2.5 g) and potassium carbonate (2 g) in acetonitrile (50 ml) was heated under reflux for 4 hours and evaporated. The residue was partitioned between ether and 2M hydrochloric acid and the acidic layer was washed with methylene chloride, basified with 10% aqueous sodium carbonate solution and extracted into methylene chloride. The organic extract was dried over magnesium sulphate and evaporated to give essentially pure 2-methyl-2-[N-(3,4-methylenedioxybenzyl)-N-methylamino]propanol as a yellow oil (2.0 g, 58%) which was used directly in Example 34. A small portion of this product was dissolved in ether and the solution was treated with excess saturated ethereal hydrogen chloride and evaporated. The residue was triturated with acetone/ethyl acetate to give the title compound as a colourless solid, m.p. 157°-159°.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 4 hours
  3. customevaporated
  4. customThe residue was partitioned between ether and 2M hydrochloric acid
  5. washthe acidic layer was washed with methylene chloride
  6. extractionextracted into methylene chloride
  7. extractionThe organic extract
  8. dry with materialwas dried over magnesium sulphate
  9. customevaporated