Ethanol → 5-(2-Ethoxyphenyl)-1-methyl-3-n-propyl-1,6-dihydro-7H-pyrazolo[4,3-d]-7-pyrimidinone

4-(2-Ethoxybenzamido)-1-methyl-3-n-propylpyrazole-5-carboxamide (223 g, 0.676 mol) was added portionwise to a solution of sodium hydroxide (54 g, 1.35 mol) and 30% hydrogen peroxide solution (224 ml) in water (2000 ml). Ethanol (700 ml) was added and the resulting mixture heated under reflux for 2.5 hours, cooled, then evaporated under vacuum. The resulting solid was treated with 2N hydrochloric acid (380 ml), with external cooling, and the mixture was extracted with dichloromethane (1×700 ml, 3×200 ml). The combined organic extracts were washed successively with saturated aqueous sodium carbonate solution (3×400 ml) and brine (300 ml), then dried (Na2SO4) and evaporated under vacuum.

1. temperaturethe resulting mixture heated
2. temperatureunder reflux for 2.5 hours
3. temperaturecooled
4. customevaporated under vacuum
5. additionThe resulting solid was treated with 2N hydrochloric acid (380 ml), with external cooling
6. extractionthe mixture was extracted with dichloromethane (1×700 ml, 3×200 ml)
7. washThe combined organic extracts were washed successively with saturated aqueous sodium carbonate solution (3×400 ml) and brine (300 ml)
8. dry with materialdried (Na2SO4)
9. customevaporated under vacuum

ORDレコード

ord-7a12599bfcb946318db19fd3111433b5

出典データセット

uspto-grants-1998_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05719283