反应详情

1.1 gm (5 meq) of dodecyl isocyanate and 726 mg (5 meq) of 6-(dimethylamino)hexanol are combined in 5 ml of tetrahydrofuran and reacted over weekend at room temperature. The insoluble crystals are filtered, washed with ethyl acetate and the filtrate and washings combined, evaporated under reduced pressure (<30° C.) and dried in vacuo. The product is purified by silica gel chromatography in the system CH2Cl2 :CH3OH:NH4OH (65:25:4). Fractions 34-46 are combined, evaporated and dried in vacuo to yield 300 mg (Rf 0.9 S.G. CH2Cl2, CH3OH, NH4OH) of title compound.

1. customreacted over weekend at room temperature
2. filtrationThe insoluble crystals are filtered
3. washwashed with ethyl acetate
4. customevaporated under reduced pressure (<30° C.)
5. customdried in vacuo
6. customThe product is purified by silica gel chromatography in the system CH2Cl2 :CH3OH:NH4OH (65:25:4)
7. customevaporated
8. customdried in vacuo