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Methanol → 2-Aminothiophene-3-carboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Cyanoacetamide | HCID 7898 | — |
| 反応物 | 1,4-Dithiane-2,5-diol | HCID 98330 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | 2-Aminothiophene-3-carboxamide | HCID 699495 | 141.7% |
反応手順
2,5-Dihydroxy-1,4-dithiane (76 g) and cyanoacetamide (84 g) were added to a mixture of methanol (180 mL), water (10 mL) and triethylamine (10 g). The resulting mixture was heated at 35–40° C. for about 30 minutes while stirring, and then heated to 50–60° C. for an additional 30 minutes with stirring. The reaction mixture was then cooled to room temperature and poured into a mixture of ice (100 g)/water (300 mL). A fine precipitate formed upon addition, which was filtered and dried overnight to give 100.6 g of the title compound as a pale gray powder ((M+H)+=143, M.P.=159.0–159.6° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07091347B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-a3cdbd0870f345c68c419ba11abf5150 |
| 出典メモ | uspto-grants-2006_08 |