反应 #83201

ord-e0d857e89cd04585803ccfc2a77737d0

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度the solution was then refluxed for 3 hours
  2. 2
    温度The reaction mixture was cooled
  3. 3
    萃取extracted with methylene chloride
  4. 4
    萃取The organic extract
  5. 5
    洗涤was washed with water
  6. 6
    其他was then collected
  7. 7
    其他dried
  8. 8
    其他evaporated to dryness
  9. 9
    其他to obtain a light amber solid (1.8 g; m.p. 113°-118° C.)

实验过程

To a freshly prepared solution of sodium ethoxide in ethanol (from 0.35 g sodium metal and 10 ml ethanol) was added 6H-pyrido[3,2,1-de]acridin-1(2H)-one (1.2 g) portionwise over a period of 10 minutes. To the resulting dark red solution was slowly added diethyl carbonate (1.77 g) and the solution was then refluxed for 3 hours. The reaction mixture was cooled, acidified to pH 2 with concentrated HCl and then extracted with methylene chloride. The organic extract was washed with water and was then collected, dried and evaporated to dryness to obtain a light amber solid (1.8 g; m.p. 113°-118° C.).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05624929uspto-grants-1997_04