反应详情

Suspend 6 gm. of the 3-cyano-8-aminodibenzo[b,f]thiepine from Example 18, Step 1, in 15 ml. of 50% fluoboric acid (HBF4) and 15 ml. of water. Cool the mixture to 3°-5° C. and slowly add 18 ml. of 10% sodium nitrite. Stir in the cold for 4 hours and add urea to destroy the excess sodium nitrite. Separate the solids by filtration and wash with cold 5% fluoboric acid followed by cold water and then ether. Air dry. Suspend the diazonium fluoroborate in 300 ml. of xylene and reflux for 2 hours with stirring. Filter and evaporate the filtrate to dryness. Triturate with ether to obtain the title product (m.p., 146°-148° C.).

1. temperatureCool the mixture to 3°-5° C.
2. customto destroy the excess sodium nitrite
3. customSeparate the solids
4. filtrationby filtration
5. washwash with cold 5% fluoboric acid
6. customAir dry
7. temperatureof xylene and reflux for 2 hours
8. stirringwith stirring
9. filtrationFilter
10. customevaporate the filtrate to dryness
11. customTriturate with ether