Benzylamine → HCID 178478160, compound
Reaction equation
[Cl:1][C:2]1[CH:3]=[C:4]([NH:8][C:9]2[C:13]([C:14]#[N:15])=[C:12]([N:16]=[CH:17][N:18](C)C)[NH:11][N:10]=2)[CH:5]=[CH:6][CH:7]=1.[CH2:21](N)[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1>>[CH2:21]([NH:15][C:14]1[N:18]=[CH:17][N:16]=[C:12]2[NH:11][N:10]=[C:9]([NH:8][C:4]3[CH:5]=[CH:6][CH:7]=[C:2]([Cl:1])[CH:3]=3)[C:13]=12)[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1Participants
3
Conditions
- Temperature
- 120 °C
Procedure
Under a nitrogen atmosphere, a mixture of 1 g (3.46 mmol) of 3-(3-chloro-phenylamino)-4-cyano-5-(dimethylamino-methyleneamino)-pyrazole and 10 ml of benzylamine is stirred for 3 hours at 120° C. and then concentrated by evaporation under a HV. The crystalline residue is digested in 10 ml of acetonitrile, cooled to 0° C. and filtered and the filter residue is recrystallized from 35 ml of acetonitrile, yielding the title compound; m.p. 216-218° C.
Workup
- concentrationconcentrated by evaporation under a HV
- temperaturecooled to 0° C.
- filtrationfiltered
- customthe filter residue is recrystallized from 35 ml of acetonitrile
Sources & evidence
- ORD record
- ord-6c193491db034e36b2e68456b258c4bf
- Source dataset
- uspto-grants-1999_11
- Patent number
- US05981533
Reaction notes
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