Triethyl orthoacetate → HCID 13533707, compound
Reaction equation
[NH:1]([C:3]1[CH:8]=[C:7]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][N:10]=2)[CH:6]=[CH:5][N:4]=1)[NH2:2].[C:15](OCC)(OCC)(OCC)[CH3:16]>>[CH3:15][C:16]1[N:4]2[CH:5]=[CH:6][C:7]([C:9]3[CH:14]=[CH:13][CH:12]=[CH:11][N:10]=3)=[CH:8][C:3]2=[N:1][N:2]=1Participants
3
Procedure
A mixture of 2.0 g of 2'-hydrazino-2,4'-bipyridine and 50 ml of triethyl orthoacetate was heated on a steam bath for 18 hours, then chilled, filtered and the crystals washed with hexane. These crystals were recrystallized from methylene chloride, giving 1.8 g of the desired product as white crystals, mp 239°-241° C.
Workup
- temperaturewas heated on a steam bath for 18 hours
- temperaturechilled
- filtrationfiltered
- washthe crystals washed with hexane
- customThese crystals were recrystallized from methylene chloride
Sources & evidence
- ORD record
- ord-9108f3fd2f154bc78e71c702367ba9e6
- Source dataset
- uspto-grants-1985_10
- Patent number
- US04550166
Reaction notes
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