Phosphorus oxychloride → HCID 59215150, compound
Reaction equation
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[N:10]=[C:11](O)[C:12]3[CH:13]=[CH:14][CH:15]=[N:16][C:17]=3[CH:18]=2)=[CH:5][CH:4]=1.O=P(Cl)(Cl)[Cl:22]>>[Cl:22][C:11]1[N:10]=[C:9]([C:6]2[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[CH:4][CH:5]=2)[CH:18]=[C:17]2[C:12]=1[CH:13]=[CH:14][CH:15]=[N:16]2Participants
3
Procedure
7-(4-Methoxyphenyl)-[1,6]naphthyridin-5-ol (13 g) and POCl3 (275 mL) was heated to 135° C. for 26 hours in a sealed tube. The mixture was cooled and the POCl3 was evaporated. The residue was poured onto ice and neutralized with 2M Na2CO3 and the precipitate was filtered and washed with H2O to yield 13.8 g of the title compound (98.5%), mp 126-127° C.
Workup
- temperatureThe mixture was cooled
- customthe POCl3 was evaporated
- additionThe residue was poured onto ice and neutralized with 2M Na2CO3
- filtrationthe precipitate was filtered
- washwashed with H2O
Sources & evidence
- ORD record
- ord-9b82c49e02a74a1484def5bbd41482e0
- Source dataset
- uspto-grants-2008_01
- Patent number
- US07321041B2
Reaction notes
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