反应 #93486

ord-cfbb51c4de9446b3ae8f6ac9ea57ff96

溶剂

反应条件

温度
90°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    萃取the mixture was extracted with ethyl acetate
  2. 2
    洗涤The extract was washed with water saturated with sodium chloride
  3. 3
    干燥dried over anhydrous sodium sulfate
  4. 4
    浓缩concentrated
  5. 5
    workup.DISSOLUTIONThe thus produced residue was dissolved in acetone
  6. 6
    workup.ADDITIONconcentrated hydrochloric acid in an amount of 2 equivalents was added
  7. 7
    其他to produce crystals
  8. 8
    过滤The crystals were filtered off

实验过程

A mixture of 2 g of 5-(5-chlorovaleryl)-2-benzyloxy-benzamide, 1 g of 1-phenylpiperazine, 0.6 g of sodium carbonate and 10 ml of dimethyl sulfoxide was heated at 90° C. for 6 hours while stirring. After the reaction was finished, water was added to the reaction mixture and the mixture was extracted with ethyl acetate. The extract was washed with water saturated with sodium chloride, dried over anhydrous sodium sulfate and concentrated. The thus produced residue was dissolved in acetone and concentrated hydrochloric acid in an amount of 2 equivalents was added thereto to produce crystals. The crystals were filtered off to obtain 2.3 g of 5-[5-(4-phenyl-1-piperazinyl)valeryl]-2-benzyloxy-benzamide (yield: 73%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04613598uspto-grants-1986_09