反应详情

A mixture of 400 mg (1.04 mmol) (R)-2-amino-3-(3,4-diethyl-phenyl)-1-[4-(1-methyl-piperidin-4-yl)-piperazin-1-yl]-propan-1-one, 205 mg (1.25 mmol) CDT, 0.2 mL (1.15 mmol) ethyldiisopropylamine and 50 mL THF was stirred for 1 h while cooling with an ice bath and stirred for 1 h at RT, then combined with 270 mg (1.11 mmol) 5-phenyl-2-piperidin-4-yl-2,4-dihydro-[1,2,4]triazol-3-one and refluxed for 4 h. The reaction mixture was evaporated down under reduced pressure, the residue was combined with saturated NaHCO3 solution and exhaustively extracted with DCM. The combined organic phases were dried, evaporated down under reduced pressure and the residue was purified by chromatography on silica gel. The product fractions were evaporated down under reduced pressure, the residue was triturated with diisopropylether, suction filtered and dried.

1. temperaturewhile cooling with an ice bath
2. stirringstirred for 1 h at RT
3. temperaturerefluxed for 4 h
4. customThe reaction mixture was evaporated down under reduced pressure
5. extractionexhaustively extracted with DCM
6. customThe combined organic phases were dried
7. customevaporated down under reduced pressure
8. customthe residue was purified by chromatography on silica gel
9. customThe product fractions were evaporated down under reduced pressure
10. customthe residue was triturated with diisopropylether, suction
11. filtrationfiltered
12. customdried