Реакция #331706

ord-b8fd1201b5654d798122c4747976812a

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ЭкстракцияThe mixture was extracted with chloroform (3×15 cm3)
  2. 2
    СушкаThe combined extracts were dried over sodium sulphate
  3. 3
    Фильтрацияfiltered
  4. 4
    Другоеthe solvent removed under reduced pressure

Методика

Methanesulphonyl chloride (838 mg, 7.35 mmol) was added slowly to a cooled solution (5° C.) of N,N-dimethyl-1,3-phenylenediamine (1.00 g, 7.35 mmol) and sodium hydroxide (5M, 1.5 cm3) in water (10 cm3). The reaction was allowed to warm to room temperature overnight. The mixture was extracted with chloroform (3×15 cm3). The combined extracts were dried over sodium sulphate, filtered and the solvent removed under reduced pressure. Column chromatography (1:20 methanol/dichloromethane) gave the target material as a brown oil (1.24 g, 79%).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08658665B2uspto-grants-2014_02