Реакция #4301

ord-95c3f93212c34abcafd8589c1a2860f7

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеThe residue obtained
  2. 2
    Экстракцияthe chloroform layer was extracted with water
  3. 3
    СушкаThe chloroform layer was dried
  4. 4
    Фильтрацияfiltered
  5. 5
    Другоеsolvent removed
  6. 6
    Другоеto give a dark brown oil
  7. 7
    ДругоеThis salt was recrystallized from methanol-diethyl ether
  8. 8
    Другоеdried 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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04724235uspto-grants-1988_02