Реакция #4301
ord-95c3f93212c34abcafd8589c1a2860f7
Уравнение реакции
Реагенты
Нет
Растворители
Условия реакции
Подробные условия
See reaction.notes.procedure_details.
Обработка
- 1ДругоеThe residue obtained
- 2Экстракцияthe chloroform layer was extracted with water
- 3СушкаThe chloroform layer was dried
- 4Фильтрацияfiltered
- 5Другоеsolvent removed
- 6Другоеto give a dark brown oil
- 7ДругоеThis salt was recrystallized from methanol-diethyl ether
- 8Другоеdried in vacuo overnight at 80° C
Методика
A solution of 105.95 g (0.456 mole) [(4-chlorobutyl)sulfonyl]benzene was heated overnight at 75° C. on an autoclave in 200 ml of isopropylamine. The reaction mixture was stripped to dryness. The residue obtained was dissolved in chloroform and the chloroform layer was extracted with water. The chloroform layer was dried, filtered, and solvent removed to give a dark brown oil. The oil was dissolved in methanol and converted to the hydrochloride salt. This salt was recrystallized from methanol-diethyl ether and dried in vacuo overnight at 80° C. This gave white crystalline product, m.p. 155°-157.5° C. in 30% yield.