反应 #502056

ord-d8f41782269540beb5e0c23e78fbed88

反应方程式

COC(=O)COc1cccc(N)c1
3-aminophenoxyacetic acid methylester
O=C([O-])[O-].[Na+].[Na+]
sodium carbonate
ClCc1ccccc1
benzyl chloride
COC(=O)COc1cccc(N(Cc2ccccc2)Cc2ccccc2)c1
3-Dibenzylaminophenoxyacetic acid methylester

反应条件

温度
100°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤The insoluble salt is filtered off
  2. 2
    洗涤washed with 100 ml of ethyl acetate
  3. 3
    workup.WAITThe combined filtrates are kept at 5° C. for 12 h
  4. 4
    萃取After the extraction with water and brine
  5. 5
    干燥the organic phase is dried with sodium sulfate
  6. 6
    其他the solvent is removed in vacuum (50° C., 10−2 mbar)

实验过程

10 g of 3-aminophenoxyacetic acid methylester are solved in 19 g benzyl chloride. Subsequently, 14 g of sodium carbonate are added portionwise and the temperature is raised to 100° C. The reaction mixture is stirred at this temperature for 3 hours. The insoluble salt is filtered off and washed with 100 ml of ethyl acetate. The combined filtrates are kept at 5° C. for 12 h. After the extraction with water and brine, the organic phase is dried with sodium sulfate and the solvent is removed in vacuum (50° C., 10−2 mbar). Yield: 22 g (dark oil).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08088182B2uspto-grants-2012_01