Реакция #502055

ord-20083fe33d1a49cbb7c1acb3fb1d8cb1

Уравнение реакции

COC(=O)COc1cccc(N)c1
3-aminophenoxyacetic acid methylester
O=C([O-])[O-].[Na+].[Na+]
sodium carbonate
C=CCN(CC=C)c1cccc(OCC(=O)OC)c1
3-Diallylaminophenoxyacetic acid methylester

Реагенты

Нет

Растворители

Условия реакции

Температура
45°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ФильтрацияThe insoluble salt is filtered off
  2. 2
    Промывкаwashed with 70 g of ethyl acetate
  3. 3
    workup.WAITThe combined filtrates are kept at 5° C. for 12 h
  4. 4
    ЭкстракцияAfter the extraction with water
  5. 5
    Сушкаthe organic phase is dried with sodium sulfate
  6. 6
    Другоеthe solvent is removed in vacuum (60° C., 28 mbar)

Методика

22 g of 3-aminophenoxyacetic acid methylester are solved in 63 g allyl bromide. Subsequently, 10 g of sodium carbonate are added portionwise and the temperature is raised to 45° C. The reaction mixture is stirred at this temperature for 4.5 hours. The insoluble salt is filtered off and washed with 70 g of ethyl acetate. The combined filtrates are kept at 5° C. for 12 h. After the extraction with water, the organic phase is dried with sodium sulfate and the solvent is removed in vacuum (60° C., 28 mbar). Yield: 24 g (dark oil).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08088182B2uspto-grants-2012_01