HRID621769

反应详情

EQUATION

反应方程式

HRID 621769 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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.

WORKUP

后处理

  1. customThe reaction mixture is evaporated under reduced pressure (<30° C.)
  2. customdried in vacuo
  3. customchromatographed 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. customevaporated under reduced pressure <30° C.
  5. customdried in vacuo