Реакция #50318

ord-4655013adc7c40efa849fa31ccac77fb

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеThe solvent was removed
  2. 2
    Экстракцияthe residue was extracted with ethyl acetate
  3. 3
    Промывкаwashed with water
  4. 4
    Сушкаdried over anhydrous magnesium sulfate
  5. 5
    ДругоеAfter removal of the solvent

Методика

A solution of N-(3-trifluoromethylphenyl)thiourea (6.1 g) , dibromoethane (5.7 g) and anhydrous potassium carbonate (11.5 g) in acetone (60 ml) was refluxed for 1 day. The solvent was removed by distillation therefrom, and the residue was extracted with ethyl ether, washed with water, dried over anhydrous magnesium sulfate and subjected to column chromatography to give 7.5 g of 2-imino-3-(3-trifluoromethylphenyl)thiazolidine. The thus obtained 2-imino-3- (3-trifluoromethylphenyl) thiazolidine (1.0 g), n-butyl chlorocarbonate (0.61 g) and triethylamine (1.2 g) were dissolved in tetrahydrofuran, and the resultant solution was stirred at room temperature for 5 hours. The solvent was removed, and the residue was extracted with ethyl acetate, washed with water and dried over anhydrous magnesium sulfate. After removal of the solvent, the residue was subjected to column chromatography to give 0.57 g of 2-butoxycarbonylimino-3- (3-trifluoromethylphenyl) thiazolidine.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05426188uspto-grants-1995_06