反应 #4471

ord-76b14a9408c64659932b886070897fcf

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    浓缩The mixture was concentrated to one half of its volume
  2. 2
    过滤The mixture was filtered off
  3. 3
    洗涤washed with water (50 ml)
  4. 4
    其他air-dried for 1 h
  5. 5
    干燥dried in vacuo over phosphorus pentoxide

实验过程

The product of Stage (ii) (7.28 g), potassium carbonate (9.90 g), acetone (70 ml), and dimethylsulphate (5.1 ml) were vigorously stirred at room temperature overnight under nitrogen. The mixture was concentrated to one half of its volume and then stirred with water (350 ml) for 30 min. The mixture was filtered off, washed with water (50 ml), air-dried for 1 h, and dried in vacuo over phosphorus pentoxide to give the title compound as needles (7.59 g), m.p. 157.5°-158.5°.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04725615uspto-grants-1988_02