Methanol → HCID 22228088, compound
Reaction equation
[Na].Cl[C:3]1[N:7]([C:8]2[CH:13]=[CH:12][C:11]([F:14])=[CH:10][CH:9]=2)[N:6]=[CH:5][C:4]=1[C:15]([NH:17][C:18]1[CH:23]=[CH:22][C:21]([O:24][CH2:25][C:26]([CH3:29])([CH3:28])[CH3:27])=[C:20]([C:30]#[N:31])[CH:19]=1)=[O:16].[I-].[K+].[CH3:34][OH:35]>>[C:30]([C:20]1[CH:19]=[C:18]([NH:17][C:15]([C:4]2[CH:5]=[N:6][N:7]([C:8]3[CH:13]=[CH:12][C:11]([F:14])=[CH:10][CH:9]=3)[C:3]=2[O:35][CH3:34])=[O:16])[CH:23]=[CH:22][C:21]=1[O:24][CH2:25][C:26]([CH3:29])([CH3:28])[CH3:27])#[N:31]Participants
5
Procedure
To a methanol solution (20 ml) containing metallic sodium (0.065 g) were added 5-chloro-N-(3-cyano-4-neopentyloxyphenyl)-1-(4-fluorophenyl)pyrazole-4-carboxamide (1 g) and a catalytic amount of potassium iodide, and the mixture was stirred at 65° C. for 5 h. The solvent was evaporated. Water was added to the residue to allow crystallization. The crystals were recrystallized from hydrous methanol to give the title compound (0.3 g), melting point: 120–123° C.
Workup
- customThe solvent was evaporated
- additionWater was added to the residue
- customcrystallization
- customThe crystals were recrystallized from hydrous methanol
Sources & evidence
- ORD record
- ord-48b560d66b0340acb67671da86f61e32
- Source dataset
- uspto-grants-2006_03
- Patent number
- US07015218B1
Reaction notes
Loading…