反应 #1687634

ord-dddecb71856e4b40b10c34c0a9991333

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度The suspension was refluxed for 4 h
  2. 2
    过滤filtered
  3. 3
    其他The toluene phase was separated
  4. 4
    萃取the aqueous phase extracted with 2×100 ml of toluene
  5. 5
    干燥The combined organic phase were dried over MgSO4
  6. 6
    其他evaporated in vacuo
  7. 7
    其他leaving a heavy, yellow oil, 88

实验过程

To a solution of 8.0 g (0.045 mol) of 73 in 125 ml of toluene, 10 g (0.045 mol) of P4S10 was added. The suspension was refluxed for 4 h and left at room temperature overnight. The mixture was poured into ice water followed by basification with ammonia. The two-phase system was stirred with charcoal and filtered. The toluene phase was separated and the aqueous phase extracted with 2×100 ml of toluene. The combined organic phase were dried over MgSO4 and evaporated in vacuo leaving a heavy, yellow oil, 88. Yield: 2.3 g (0.013 mol), 29%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: USRE036374uspto-grants-1999_11