反应详情

A mixture of 5-chloro-2-phenyl-7,8,9,10-tetrahydro-1,2,4-triazolo[4,3-c]quinazolin-3-one (150 mg, 0.5 mmol), diisopropylethylamine (130 ml, 0.74 mmol) and 10% Pd-C (30 mg) was hydrogenated under H2 balloon for 1 hour. The reaction was filtered through Celite. NaBH4 (30 mg, 0.79 mmol) was added to the filtrate and the mixture was heated to reflux temperature. The reaction was poured into water and extracted with CH2Cl2 (3×50 ml). The combined organic layers were dried over Na2SO4 and evaporated under reduced pressure. The residue was triturated with ethanol and filtered to afford 2-phenyl-5,6,7,8,9,10-hexahydro-1,2,4-triazolo[4,3-c]-quinazolin-3-one (Compound 31), m.p. 158-159° C.

1. customfor 1 hour
2. filtrationThe reaction was filtered through Celite
3. temperaturethe mixture was heated
4. temperatureto reflux temperature
5. extractionextracted with CH2Cl2 (3×50 ml)
6. dry with materialThe combined organic layers were dried over Na2SO4
7. customevaporated under reduced pressure
8. customThe residue was triturated with ethanol
9. filtrationfiltered