Valeryl chloride → HCID 21246379, compound
Reaction equation
Cl.[NH:2]=[C:3]1[CH:8]=[CH:7][N:6]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[N:5]=[CH:4]1.[C:15]([Cl:21])(=[O:20])[CH2:16][CH2:17][CH2:18][CH3:19]>>[ClH:21].[C:9]1([N:6]2[CH:7]=[CH:8][C:3](=[N:2][C:15](=[O:20])[CH2:16][CH2:17][CH2:18][CH3:19])[CH:4]=[N:5]2)[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1Participants
3
Procedure
6.0 g (28.9 millimoles) of 1,4-dihydro-4-imino-1-phenylpyridazine hydrochloride in 40 ml of valeryl chloride were kept at 120° C. for 20 hours, while stirring. The mixture was cooled and then filtered under suction, and the residue was washed with acetone and recrystallized first from ethanol/methyl tert.-butyl ether and then from ethanol/acetone. 3.4 g (40% of theory) of 1,4-dihydro-1-phenyl-4-(valerylimino)-pyridazine hydrochloride were isolated as pale yellowish crystals of melting point 180°-182° C.
Workup
- temperatureThe mixture was cooled
- filtrationfiltered under suction
- washthe residue was washed with acetone
- customrecrystallized first from ethanol/methyl tert.-butyl ether
Sources & evidence
- ORD record
- ord-4defbb777486401eafeb0b252b83ab6e
- Source dataset
- uspto-grants-1989_04
- Patent number
- US04820821
Reaction notes
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