Реакция #2006463
ord-6ecfca2cb2f4480d83dd78ee9f3ae4c0
Уравнение реакции
sodium hydroxide
tert-butylcarbamidine hydrochloride
trichloromethanesulphenyl chloride
→
3-(tert-Butyl)-5-chloro-1,2,4-thiadiazole
Выход 60.0%
Реагенты
Нет
Растворители
Условия реакции
Температура
-15°CELSIUS
Подробные условия
See reaction.notes.procedure_details.
Обработка
- 1Другоеthe mixture obtained
- 2Экстракцияextracting three times with water
- 3Сушкаdrying the combined organic phases over MgSO4
- 4Другоеthe solvent is evaporated under vacuum
Методика
6.83 g (50.00 mmol) of tert-butylcarbamidine hydrochloride are dissolved in 60 ml of dichloromethane and treated with 8.37 g (45.00 mmol) of trichloromethanesulphenyl chloride, before the reaction mixture is cooled to −15° C. A solution of 10.00 g (250 mmol) of sodium hydroxide in 20 ml of water is added dropwise and the mixture obtained is stirred at AT for 3 h. After adding 50 ml of dichloromethane, extracting three times with water and drying the combined organic phases over MgSO4, the solvent is evaporated under vacuum. (5.81 g, 90% purity, 60% yield, log P (pH 2.3)=3.44).