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Potassium Carbonate → N-benzyloxy-3-chloropropylsulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-Chloropropanesulphonyl chloride | HCID 15410 | — |
| 反応物 | Benzyloxyamine hydrochloride | HCID 102312 | — |
| 触媒 | Bis(tetrabutylammonium) sulphate | HCID 11433187 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | N-benzyloxy-3-chloropropylsulfonamide | HCID 10539517 | 41% |
反応手順
3-Chloropropylsulfonyl chloride 1 (30.28 g,0.17 mol), O-benzylhydroxylamine hydrochloride (27.3 g,0.17 mol), potassium carbonate (50 g,0.36 mol) and tetrabutylammonium sulfate (about 500 mg) are reacted with each other in a mixture of ether and water (1:1) (100 ml) for 24 hours at room temperature and the reaction mixture was extracted with ethyl acetate. The extract was subjected to column chromatography on silica gel. From the fraction eluted with a mixture of ethyl acetate/n-hexane (1:4),18.4 g (41%) of crude N-benzyloxy-3-chloropropylsulfonamide (intermediate 3g) was obtained as a pale yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05418230 |
| 出典データセット | uspto-grants-1995_05 |
| ORD ID | ord-ffa5db23b6c645ea926f7c0af8d36b34 |
| 出典メモ | uspto-grants-1995_05 |