Реакция #708951

ord-01ab017c257f415c9679c2afc28f6aec

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеThe reaction mixture is evaporated under reduced pressure (<30° C.)
  2. 2
    Другоеdried in vacuo
  3. 3
    Другоеchromatographed on silica gel in the system CH2Cl2 :CH3OH:NH4OH (65:25:4) and fractions 47-52 having Rf 0.9 on TLC S.G
  4. 4
    Другоеevaporated under reduced pressure <30° C.
  5. 5
    Другоеdried in vacuo

Методика

650 mg (2 meq) of hexadecanesulfonylchloride are added dropwise to 744 mg (4 meq) of 7-dimethylaminoheptylamine stirring in tetrahydrofuran at 0° C. The reaction mixture is evaporated under reduced pressure (<30° C.) dried in vacuo, and chromatographed on silica gel in the system CH2Cl2 :CH3OH:NH4OH (65:25:4) and fractions 47-52 having Rf 0.9 on TLC S.G. CH2Cl2 :CH3OH:NH4OH are combined, evaporated under reduced pressure <30° C. and dried in vacuo to yield 300 mg of title compound having a m.p. of 56°-57.5° C. uncorr.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04824996uspto-grants-1989_04