1,1'-Biphenyl, mixt. with 1,1'-oxybis(benzene) → HCID 20040895, compound
Reaction equation
[CH3:1][C:2]1[N:3]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[N:4]=[CH:5][C:6]=1[NH:7]/[C:8](/[CH3:15])=[CH:9]\[C:10]([O:12]CC)=O.C1C=CC(C2C=CC=CC=2)=CC=1.C1C=CC(OC2C=CC=CC=2)=CC=1>>[O:12]=[C:10]1[CH:9]=[C:8]([CH3:15])[NH:7][C:6]2=[C:2]([CH3:1])[N:3]([C:16]3[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=3)[N:4]=[C:5]12Participants
3
Procedure
Ethyl 3-(3-methyl-2-phenylpyrazol-4-ylamino)crotonate (0.200 g) was added to boiling Dowtherm A (5 ml) under nitrogen. The mixture was heated under reflux for 30 mins and then allowed to cool. Petroleum ether (60°-80° C.) was added to the cooled Dowtherm solution and the required pyrazolopyridone precipitated out. The title compound (0.120 g) was filtered off and washed thoroughly with hot petroleum ether.
Workup
- temperatureThe mixture was heated
- temperatureunder reflux for 30 mins
- temperatureto cool
- customthe required pyrazolopyridone precipitated out
- filtrationThe title compound (0.120 g) was filtered off
- washwashed thoroughly with hot petroleum ether
Sources & evidence
- ORD record
- ord-7c2c66c5cbb347e5a9dff2ed2a2470cb
- Source dataset
- uspto-grants-1989_05
- Patent number
- US04833136
Reaction notes
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