反应详情

温度

100 °C

A mesyl compound (Example 3, 1 g) and sodium azide were added to dimethylformamide (20 ml), and the mixture was stirred at 100° C. for 50 minutes. After completion of the reaction, pressure was reduced to concentrate the mixture. The concentrate was diluted with a solvent mixture of chloroform and methanol (5:1), washed with water, and dried. When the solvent was evaporated, 759 mg of the title compound was obtained (91.6%). This substance was recrystallized from a solvent mixture of chloroform-n-hexane, obtaining yellow powdery crystals having a melting point of 192°-194° C.(dec.).

1. customAfter completion of the reaction, pressure
2. concentrationto concentrate the mixture
3. additionThe concentrate was diluted with a solvent mixture of chloroform and methanol (5:1)
4. washwashed with water
5. customdried
6. customWhen the solvent was evaporated