Реакция #586102

ord-8875f359d9d14de7b83db0f79e1bddf3

Уравнение реакции

CCC(C)(C)c1cccc(NC=O)c1C
N-(2-methyl-3-(1,1-dimethylpropyl)phenyl)form-amide
[K+].[OH-]
potassium hydroxide
CO
methanol
CCC(C)(C)c1cccc(N)c1C
3-(1,1-dimethypropyl)-2-methyl-phenylamine

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураat reflux temperature for 15 hours
  2. 2
    workup.ADDITIONis added
  3. 3
    Экстракцияthe reaction mixture is extracted with ethylacetate
  4. 4
    СушкаAfter drying of the organic phase over sodium sulfate and evaporation of the solvent in a water jet vacuum
  5. 5
    Другоеthe product is purified by destillation (bp. ca. 70° C., 13,33 Pa)

Методика

2,21 g (10.77 mmol) N-(2-methyl-3-(1,1-dimethylpropyl)phenyl)form-amide, 1,42 g (21.54 mmol) 85% potassium hydroxide and 9 ml methanol are heated under stirring at reflux temperature for 15 hours. After cooling 100 ml of water is added and the reaction mixture is extracted with ethylacetate. After drying of the organic phase over sodium sulfate and evaporation of the solvent in a water jet vacuum, the product is purified by destillation (bp. ca. 70° C., 13,33 Pa). This gives 1.7 g of 2-Methyl-3-(1,1-dimethylpropyl)phenylamine in the form of a colourless oil (89% of theory).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07767625B2uspto-grants-2010_08