反应详情

1-(4-Methanesulphonamidophenyl)-4-(4-methanesulphonamidophenacyl)piperazine [see Example 5(D)] (0.77 g) was dissolved in ethanol (3 ml) and dimethylformamide (5 ml). Sodium borohydride (0.125 g) was then added portionwise over 5 minutes, and the mixture was stirred for 21/2 hours at ambient temperature. A further 25 mg. sodium borohydride was then added and the reaction mixture was heated at 60° for 2 hours. A further 20 mg. of borohydride was added, and the reaction mixture was heated at 70° for 41/2 hours. The mixture was then diluted with water, precipitating the impure product containing some unreduced starting material (0.51 g after drying). This impure product was refluxed for 41/2 hours in ethanol (35 ml), adding sodium borohydride (110 mg) portionwise during the first 2 hours. The mixture was then evaporated, the residue washed with water, and crystallized from methanol, yield of the pure title compound 0.118 g., m.p. 230°-2° (dec.).

1. temperaturethe reaction mixture was heated at 60° for 2 hours
2. temperaturethe reaction mixture was heated at 70° for 41/2 hours
3. customprecipitating the impure product
4. additioncontaining
5. customsome unreduced starting material (0.51 g after drying)
6. temperatureThis impure product was refluxed for 41/2 hours in ethanol (35 ml)
7. additionadding sodium borohydride (110 mg) portionwise during the first 2 hours
8. customThe mixture was then evaporated
9. washthe residue washed with water
10. customcrystallized from methanol, yield of the pure title compound 0.118 g