Dimethylformamide diethylacetal → HCID 54299500, compound
Reaction equation
[C:1]([C:4]1[CH:5]=[CH:6][C:7]([Cl:10])=[N:8][CH:9]=1)(=[O:3])[CH3:2].C(O[CH:14](OCC)[N:15]([CH3:17])[CH3:16])C>>[CH3:14][N:15]([CH3:17])[CH:16]=[CH:2][C:1]([C:4]1[CH:5]=[CH:6][C:7]([Cl:10])=[N:8][CH:9]=1)=[O:3]Participants
3
Procedure
15.4 g (98.7 mmol) of 5-acetyl-2-chloro-pyridine are stirred for 1 h at 110° with 100 ml of dimethylformamide diethylacetal. After cooling to 0° filtering and drying at 60°, under HV, 3-dimethylamino-1-(2-chloro-5-pyridyl)-2-propen-1-one is obtained; 1H-NMR (DMSO): 2.98 (3H,s), 3.2 (3H,s), 5.9 (1H,d), 7.6 (1H,d), 7.8 (1H,d), 8.3 (1H, m), 8.9 (1H,m).
Workup
- temperatureAfter cooling to 0°
- filtrationfiltering
- customdrying at 60°, under HV
Sources & evidence
- ORD record
- ord-a6cc567307f74b2097104c4811b0a320
- Source dataset
- uspto-grants-1997_03
- Patent number
- US05612340
Reaction notes
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