Phosphorus oxychloride → 3,5-Dichloro-benzofuro[3,2-c]isoquinoline
反応式
[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]3[O:15][C:14]4[CH:16]=[CH:17][CH:18]=[CH:19][C:13]=4[C:7]=3[N:8]=[C:9]2O)=[CH:4][CH:3]=1.O=P(Cl)(Cl)[Cl:22]>>[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]3[O:15][C:14]4[CH:16]=[CH:17][CH:18]=[CH:19][C:13]=4[C:7]=3[N:8]=[C:9]2[Cl:22])=[CH:4][CH:3]=1参加物
3
実験手順
A mixture of 19B (11.8 mmol) in POCl3 (20 mL) was refluxed for 2 hours. After reaction completed, POCl3 was evaporated under reduced pressure. The residue was added into crushed ice and stirred for 10 min. The solids were collected by filtration and dried to give 3.2 g of a crude product, which was dissolved in dichloromethane and purified by flash chromatography (petroleum ether 1:1) and concentrated to give a pure product M19 (3.1 g).
後処理
- temperaturewas refluxed for 2 hours
- customAfter reaction
- customPOCl3 was evaporated under reduced pressure
- additionThe residue was added
- custominto crushed ice
- filtrationThe solids were collected by filtration
- customdried
出典と根拠
- ORDレコード
- ord-573149b925c84f3da98822107018f8eb
- 出典データセット
- uspto-grants-2015_03
- 特許番号
- US08969373B2
反応ノート
読み込み中…