HRID1948613

反应详情

EQUATION

反应方程式

HRID 1948613 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

[8-(3-methoxypropyl)-1,4-dioxa-spiro[4.5]dec-8-yl]-dimethylamine (8.11 g, 31.5 mmole) was dissolved in water (12 ml), conc. HCl (19.5 ml) was added while cooling with ice, and the reaction mixture was stirred for 3 days at room temperature. The reaction mixture was washed with ether (2×75 ml). The solution was then made alkaline with 5N NaOH and extracted with dichloromethane (3×75 ml). The combined organic phases were washed with water (75 ml), dried over Na2SO4, filtered, and the solvent was removed in vacuo.

WORKUP

后处理

  1. temperaturewhile cooling with ice
  2. washThe reaction mixture was washed with ether (2×75 ml)
  3. extractionextracted with dichloromethane (3×75 ml)
  4. washThe combined organic phases were washed with water (75 ml)
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. customthe solvent was removed in vacuo