Phosphorus pentachloride → heptane-1-sulfonyl chloride
反応式
P(Cl)(Cl)(Cl)(Cl)[Cl:2].[CH2:7]([S:14]([OH:17])(=O)=[O:15])[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH3:13].[Na]>>[CH2:7]([S:14]([Cl:2])(=[O:17])=[O:15])[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH3:13]参加物
4
実験手順
To phosphorous pentachloride (3.3 g, 16 mmol) was added solid heptanesulfonic acid, sodium salt monohydrate (1.75 g, 8 mmol) and the mixture was left to stir overnight under nitrogen. Phosphorous oxychloride was removed by distillation at 150° C. for 3 h. The residue was distilled under reduced pressure (ca. 5 mm Hg) at 135° C. to give ca. 1 g of material which was allowed to cool to room temperature. The precipitated free acid was removed by filtration to afford the title compound as an oil (500 mg, 31%) which was used without further purification.
後処理
- waitthe mixture was left
- customPhosphorous oxychloride was removed by distillation at 150° C. for 3 h
- distillationThe residue was distilled under reduced pressure (ca. 5 mm Hg) at 135° C.
出典と根拠
- ORDレコード
- ord-99f74e0b64e84e4dad4737a1816ed3d2
- 出典データセット
- uspto-grants-2003_08
- 特許番号
- US06610711B2
反応ノート
読み込み中…