関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Phosphorus sulfide (P2S5) | HCID 14817 | — |
| 反応物 | 2,2-Diethoxyacetamide | HCID 100765 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2,2-Diethoxythioacetamide | HCID 2794734 | 66.1% |
反応手順
To a suspension of phosphorus pentasulfide (27 g) in dry THF (100 ml) at 0° C. under vigorous stirring, Na2CO3 (13 g) was added. The reaction mixture was stirred for 30 min at 0° C. and for 30 min at r.t., then diethoxyacetamide (6 g) was added and stirring was continued at r.t. for 70 h. The reaction was then diluted with EA, washed with 10% Na3PO4, brine, dried over Na2SO4 and the solvent removed in vacuo. The crude residue was purified by flash-chromatography (EE/PE 1/1) to give the title compound as a white solid (4.4 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06531466B2 |
|---|
| 出典データセット | uspto-grants-2003_03 |
|---|
| ORD ID | ord-037d3a3fce9b483eb552b0c43bec90a2 |
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| 出典メモ | uspto-grants-2003_03 |
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