Phosphorus oxychloride → HCID 86722242、化合物
反応式
O[C:2]1[CH:7]=[C:6]([C:8]2[N:9]=[C:10]([CH:13]([CH3:15])[CH3:14])[S:11][CH:12]=2)[N:5]=[C:4]2[C:16]3[C:22]([Cl:23])=[C:21]([O:24][CH3:25])[CH:20]=[CH:19][C:17]=3[O:18][C:3]=12.O=P(Cl)(Cl)[Cl:28]>>[Cl:28][C:2]1[CH:7]=[C:6]([C:8]2[N:9]=[C:10]([CH:13]([CH3:15])[CH3:14])[S:11][CH:12]=2)[N:5]=[C:4]2[C:16]3[C:22]([Cl:23])=[C:21]([O:24][CH3:25])[CH:20]=[CH:19][C:17]=3[O:18][C:3]=12参加物
3
実験手順
The crude 10C (8.75 g, 23.34 mmol) was added to POCl3 (200 mL) The mixture was refluxed for 2 hours. TLC monitored the reaction. After the reaction completed, POCl3 was evaporated under reduced pressure. The residue was poured into crushed ice under stirring. The yellow solids were collected by filtration and purified by flash chromatography to give product M10 (0.66 g).
後処理
- temperaturewas refluxed for 2 hours
- customthe reaction
- customPOCl3 was evaporated under reduced pressure
- additionThe residue was poured
- custominto crushed ice
- filtrationThe yellow solids were collected by filtration
- custompurified by flash chromatography
- customto give product M10 (0.66 g)
出典と根拠
- ORDレコード
- ord-a8a8e91967864ef4b21bc3073a0eac08
- 出典データセット
- uspto-grants-2015_03
- 特許番号
- US08969373B2
反応ノート
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