Реакция #51667

ord-ffe6f370f9a649a1b163cc5fc18bcff1

Условия реакции

Температура
120°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураheated in an oil bath
  2. 2
    workup.STIRRINGThe homogeneous solution was stirred at this temperature for 90 minutes
  3. 3
    Температураto cool to room temperature
  4. 4
    ДругоеThe flask was immersed in an ice bath
  5. 5
    workup.ADDITIONthe suspension of the product
  6. 6
    workup.STIRRINGwas stirred at this temperature until all was crystalline
  7. 7
    ФильтрацияFiltration
  8. 8
    Промывкаwashing well with water
  9. 9
    Другоеthorough drying

Методика

The crystalline N-(2-Chloro-6-methanesulfonylmethyl-phenyl)-2,2,2-trifluoro-acetamide of Step 3 was taken up into 200 ml of 2N solution of sodium hydroxide and stirred and heated in an oil bath heated to 120° C. The homogeneous solution was stirred at this temperature for 90 minutes and slowly allowed to cool to room temperature. The flask was immersed in an ice bath and the suspension of the product was stirred at this temperature until all was crystalline. Filtration, washing well with water and thorough drying afforded 13.96 g of pure crystalline 2-chloro-6-methanesulfonylmethyl-phenylamine (90%).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US06852726B2uspto-grants-2005_02