反应详情

To a solution of β-alanine (56 mg) and sodium bicarbonate (84 mg) in water (10 ml) were added tetrahydrofuran (20 ml) and cholesterol chlorocarbonate (449 mg) at 0° C. The mixture was stirred for 1 hour. The reaction mixture was concentrated in vacuo and to the residue were added 0.1N hydrochloric acid (10 ml) and chloroform (40 ml). Organic layer was separated, washed with water and dried over magnesium sulfate. Evaporation of the solvent gave a crude product, which was dissolved in chloroform and applied to a silica gel column (40 g). Elution with a mixture of chloroform and methanol gave N-(cholest-5-en-3β-oxycarbonyl)-β-alanine (187 mg) as a white powder.

1. concentrationThe reaction mixture was concentrated in vacuo and to the residue
2. additionwere added 0.1N hydrochloric acid (10 ml) and chloroform (40 ml)
3. customOrganic layer was separated
4. washwashed with water
5. dry with materialdried over magnesium sulfate
6. customEvaporation of the solvent
7. customgave a crude product, which
8. washElution
9. additionwith a mixture of chloroform and methanol