HRID1829183

反应详情

EQUATION

反应方程式

HRID 1829183 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Sodium hydride (2.2 g, 80% dispersion in mineral oil, 73.2 mmol) was added to an ice-cooled solution of (3R)-N-tert-butoxycarbonylpyrrolidin-3-ol (J. Med. Chem. 41; 25; 1998; 4983) (12.5 g, 66.7 mmol) in tetrahydrofuran (330 ml), and the solution stirred at room temperature for an hour. Methyl iodide (14.5 g, 100 mmol) was then added and the reaction stiired for 18 hours. Water (100 ml) was added and the mixture concentrated under reduced pressure to remove the organic solvents. The aqueous was extracted with ethyl acetate, the combined organic solutions dried (MgSO4) and evaporated under reduced pressure to give the title compound as an oil, 12.48 g.

WORKUP

后处理

  1. concentrationthe mixture concentrated under reduced pressure
  2. customto remove the organic solvents
  3. extractionThe aqueous was extracted with ethyl acetate
  4. dry with materialthe combined organic solutions dried (MgSO4)
  5. customevaporated under reduced pressure