関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Cyanophenol | HCID 13019 | — |
| 反応物 | 4H,5H,6H,7H-thieno(2,3-c)pyridine | HCID 12337025 | — |
| 反応物 | HCID 178486302 | HCID 178486302 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | Isopropyl alcohol isopropyl ether | HCID 21202047 | 23% |
反応手順
A mixture of 4,5,6,7-tetrahydro-thieno[2,3-c]pyridine (1 g; 7.2 mmoles), p-cyano-phenol (95% purity; 0.9 g; 7.2 mmoles), polyoxymethylene (0.43 g; 14.4 mmoles) and dioxan (20 cc) is stirred at 80° C. during 4 hours. After concentration in vacuo, the residue is taken up into 2N hydrochloric acid. The aqueous phase is extracted with ether, made basic with concentrated ammonia and again extracted with methylene chloride. The organic extracts are washed with water, dried over sodium sulfate and concentrated in vacuo. The residue is recrystallized from isopropyl ether-isopropanol (M.p. 134° C.; yield: 23%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04163852 |
|---|
| 出典データセット | uspto-grants-1979_08 |
|---|
| ORD ID | ord-7fefc21f9657424996b491b80f457b88 |
|---|
| 出典メモ | uspto-grants-1979_08 |
|---|
