Phosphorus oxychloride → 2,6-Dichloroquinoline
反応式
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[C:7](O)[CH:6]=[CH:5]2.O=P(Cl)(Cl)[Cl:15]>>[Cl:15][C:7]1[CH:6]=[CH:5][C:4]2[C:9](=[CH:10][CH:11]=[C:2]([Cl:1])[CH:3]=2)[N:8]=1参加物
3
実験手順
180 mg 6-chloro-2-hydroxy quinoline was treated by 3 ml POCl3, the mixture was refluxed for 3 hours, the remaining POCl3 was evaporated out. After cooling to room temperature, the residue was treated by cold water, the solid was filtered out and dried as green powder, yield: 90%. Following the general procedure in claim 5, the listed compounds were achieved. Mass calculated for C9H5Cl2N: 198; LCMS: 200.1 (M+2)+; 1HNMR (400 MHZ), DMSO-d6) δ ppm 8.04 (1H, d, J=7.8 Hz), 7.97 (1H, d, J=8.8 Hz), 7.81 (1H, d, J=1.9 Hz), 7.68 (1H, dd, J=9.8 Hz, J=2.9 Hz), 7.42 (1H, d, J=8.8 Hz).
後処理
- temperaturethe mixture was refluxed for 3 hours
- customthe remaining POCl3 was evaporated out
- additionthe residue was treated by cold water
- filtrationthe solid was filtered out
- customdried as green powder, yield: 90%
出典と根拠
- ORDレコード
- ord-8ab2125dfc3e4565887e933bdb194c31
- 出典データセット
- uspto-grants-2013_06
- 特許番号
- US08455516B2
反応ノート
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