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Ethyl Acetate → 2,2-Diethoxythioacetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 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 | — |
| 生成物 | 2,2-Diethoxythioacetamide | HCID 2794734 | 90.2% |
反応手順
To a stirred mixture of P2S5 (45 g) in THF (300 ml) at 23°, sodium carbonate (21.5 g) was added. At the mixture, vigorously stirred, 2,2-diethoxyacetamide (10 g) was added. After 24 h a 10% aqueous solution of Na3PO4 (200 ml), EA (300 ml) and CH (300 ml) were respectively added. The aqueous layer was washed with EA and united to the organic layer. This was washed with water until clarification, dried and the solvent evaporated under reduce pressure. The crude residue was purified by flash chromatography (eluting with CH-EA 1:1) to give the title compound as a white solid (10 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-fa9db38bfdff4928a25e16fdd5ca99f6 |
| 出典メモ | uspto-grants-2003_03 |