Реакция #1884962
ord-898e242162d8486fb5e3eaee4ead7238
Уравнение реакции
tert-Butylamine
3-Chloropropanesulfonyl chloride
→
product
Выход 99.0%
N-tert-Butyl-(3-chloro)propylsulfonamide
Выход 99.0%
Реагенты
Нет
Растворители
Условия реакции
Подробные условия
See reaction.notes.procedure_details.
Обработка
- 1ТемператураThe solution was cooled to −200C
- 2ФильтрацияThe mixture was filtered
- 3Концентрированиеthe filtrate was concentrated in vacuo
- 4workup.DISSOLUTIONThe residue was dissolved in CH2Cl2 (2.0 L)
- 5ПромывкаThe resulting solution was washed with 1 N HCl (1.0 L), water (1.0 L), brine (1.0 L)
- 6Сушкаdried over Na2SO4
- 7ФильтрацияIt was filtered
- 8Концентрированиеconcentrated in vacuo
- 9Другоеto give a slightly yellow solid, which
- 10Другоеwas crystallized from hexane
Методика
tert-Butylamine (3.0 mol, 315.3 mL) was dissolved in THF (2.5 L). The solution was cooled to −200C. 3-Chloropropanesulfonyl chloride (1.5 mol, 182.4 mL) was added slowly. The reaction mixture was allowed to warm to rt and stirred for 24 h. The mixture was filtered, and the filtrate was concentrated in vacuo. The residue was dissolved in CH2Cl2 (2.0 L). The resulting solution was washed with 1 N HCl (1.0 L), water (1.0 L), brine (1.0 L) and dried over Na2SO4. It was filtered and concentrated in vacuo to give a slightly yellow solid, which was crystallized from hexane to afford the product as a white solid (316.0 g, 99%).