Methanol → HCID 18980921, compound
Reaction equation
[F:1][C:2]([F:29])([F:28])[C:3]1[CH:8]=[CH:7][C:6]([NH:9][C:10]([N:12]2[CH2:16][C:15]([N:18]=[C:19]=[O:20])([CH3:17])[C:14]([C:21]3[CH:26]=[CH:25][C:24]([Cl:27])=[CH:23][CH:22]=3)=[N:13]2)=[O:11])=[CH:5][CH:4]=1.[CH3:30][OH:31]>>[F:29][C:2]([F:1])([F:28])[C:3]1[CH:8]=[CH:7][C:6]([NH:9][C:10]([N:12]2[CH2:16][C:15]([NH:18][C:19]([O:31][CH3:30])=[O:20])([CH3:17])[C:14]([C:21]3[CH:22]=[CH:23][C:24]([Cl:27])=[CH:25][CH:26]=3)=[N:13]2)=[O:11])=[CH:5][CH:4]=1Participants
3
Procedure
A solution of 20 g (47 mmole) of N-(4-trifluoromethylphenyl)-3-(4-chlorophenyl)-4-isocyanato-4-methyl-4,5-dihydro-1H-pyrazole-1-carboxamide (Example 1d) in 200 ml of methanol was refluxed for 2 hours, concentrated in vacuo and recrystallized from ethyl acetate/hexanes yielding 19.8 g (92%) of a white solid, mp 179°-181° C.
Workup
- concentrationconcentrated in vacuo
- customrecrystallized from ethyl acetate/hexanes yielding 19.8 g (92%) of a white solid, mp 179°-181° C.
Sources & evidence
- ORD record
- ord-ebf7c5b208e54388bf7100d937045ac0
- Source dataset
- uspto-grants-1998_08
- Patent number
- US05798311
Reaction notes
Loading…