HCID 836063, compound → HCID 11805638, compound
Reaction equation
[C:1]([NH:9][C:10]1[C:11](Cl)=[N:12][CH:13]=[CH:14][CH:15]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C[Si](OP(=O)=O)(C)C>>[C:2]1([C:1]2[O:8][C:11]3[C:10]([N:9]=2)=[CH:15][CH:14]=[CH:13][N:12]=3)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1Participants
3
Procedure
1.9 g (8 mmol) of 3-benzoylamino-2-chloropyridine, prepared in stage A, are added to the PPSE solution and then brought to reflux for 15 hours. The 1,2-dichlorobenzene is then evaporated off under vacuum. The residue is treated with a water/ice mixture. The pH of the solution is adjusted to 7-8 with 5% sodium bicarbonate solution. The precipitated product is filtered off and then recrystallized in cyclohexane.
Workup
- temperatureto reflux for 15 hours
- customThe 1,2-dichlorobenzene is then evaporated off under vacuum
- additionThe residue is treated with a water/ice mixture
- filtrationThe precipitated product is filtered off
- customrecrystallized in cyclohexane
Sources & evidence
- ORD record
- ord-0933c67cb8884196afc3fb36c86ef009
- Source dataset
- uspto-grants-1991_12
- Patent number
- US05077408
Reaction notes
Loading…