反应详情

温度

3 °C

Suspend 50 mg. of the 3-cyano-8-aminodibenzo[b,f]thiepine from Example 18, Step 1, in 2 ml. of 10% sulfuric acid and cool to 3° C. Add dropwise 0.2 ml. of 10% aqueous sodium nitrite solution. Stir at 3° C. for 2 hours and allow to warm to 15° C. for 1 hour. Add the solution dropwise to 50 ml. of boiling 10% sulfuric acid and continue heating for 15 minutes. Dilute with cold water and filter. Wash the solids with water and dry to obtain the title product (m.p., 224°-227° C.).

1. additionAdd dropwise 0.2 ml
2. temperatureto warm to 15° C. for 1 hour
3. additionAdd the solution dropwise to 50 ml
4. temperaturecontinue heating for 15 minutes
5. filtrationfilter
6. washWash the solids with water
7. customdry