Reaction equation
[ClH:1].[CH2:2]([C:4]1[N:8]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[C:7]([C:15]2[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[CH:17][CH:16]=2)=[N:6][N:5]=1)[CH3:3].C(OC(C)C)(C)C>C(O)C>[ClH:1].[CH2:2]([C:4]1[N:8]([C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=2)[C:7]([C:15]2[CH:16]=[CH:17][C:18]([O:21][CH3:22])=[CH:19][CH:20]=2)=[N:6][N:5]=1)[CH3:3]Participants
5
Procedure
2.85 ml of a 6.4N hydrogen chloride solution in ethanol were added to a solution of 5.1 g of the product of Example 6 in 5.1 ml of ethanol and then isopropyl ether was added thereto. The mixture was filtered and the recovered product was empasted several times with isopropyl ether, filtered and was dried. The product was dissolved in 350 ml of tetrahydrofuran and the solution was filtered and concentrated to a volume of 75 ml. The mixture was cooled, iced and filtered and the recovered product was washed with tetrahydrofuran and dried to obtain 3.3 g of 3-ethyl-5-(4-methoxyphenyl)-4-phenyl-4H-1,2,4-triazole hydrochloride melting towards 150° C. with decomposition.
Workup
- filtrationThe mixture was filtered
- filtrationfiltered
- customwas dried
- dissolutionThe product was dissolved in 350 ml of tetrahydrofuran
- filtrationthe solution was filtered
- concentrationconcentrated to a volume of 75 ml
- temperatureThe mixture was cooled
- filtrationiced and filtered
- washthe recovered product was washed with tetrahydrofuran
- customdried
Sources & evidence
- ORD record
- ord-62c3bd1087044bac95b710b6c602a40b
- Source dataset
- uspto-grants-1987_04
- Patent number
- US04659729
Linked notes
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