反应详情

温度

145 °C

A suspension of 3-aminopyrazole-4-carboxamide hemisulphate (113 g.) in formamide (325 ml.) was stirred and heated to 145° C. The reaction was held at 145° C. for 5 hours. The reaction was then cooled to 30° C. and the product collected and washed with formamide (2 × 50 ml.), water (2 × 150 ml.) and acetone (2 × 100 ml.). Wt. of crude product = 79 gms. The crude product was recrystallized by dissolution in a solution made from sodium hydroxide (25 g.) in water (1200 ml.) with treatment at 25° C. with charcoal (8 g.), followed by reprecipitation by the addition of concentrated hydrochloric acid to pH 5. The product was collected and washed with cold water (2 × 300 ml.), acetone (2 × 200 ml.) and dried in vacuo at 60° C. Weight = 70 g. Yield = 80%.

1. temperatureThe reaction was then cooled to 30° C.
2. customthe product collected
3. washwashed with formamide (2 × 50 ml.), water (2 × 150 ml.) and acetone (2 × 100 ml.)
4. customThe crude product was recrystallized by dissolution in a solution
5. custommade from sodium hydroxide (25 g.) in water (1200 ml.) with treatment at 25° C. with charcoal (8 g.)
6. customfollowed by reprecipitation by the addition of concentrated hydrochloric acid to pH 5
7. customThe product was collected
8. washwashed with cold water (2 × 300 ml.), acetone (2 × 200 ml.)
9. customdried in vacuo at 60° C