関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Oxalic Acid | HCID 971 | — |
| 反応物 | 4-Nitrophenol | HCID 980 | — |
| 反応物 | 1,4-Dioxane | HCID 31275 | — |
| 反応物 | 6-Methyl-4,5,6,7-tetrahydrothieno[3,2-c]pyridine | HCID 20321991 | — |
| 反応物 | HCID 178486302 | HCID 178486302 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 5-(2-Hydroxy-5-nitro-benzyl)-6-methyl-4,5,6,7-tetrahydro-thieno[3,2-c]pyridine | HCID 20396037 | 27% |
反応手順
A mixture of 6-methyl-4,5,6,7-tetrahydro-thieno[3,2-c]pyridine (6.3 g; 41 mmoles), p-nitro-phenol (5.7 g; 41 mmoles), polyoxymethylene (2.5 g; 83 mmoles) and dioxan (50 cc) is stirred at 80° C. during 4 hours. After concentration in vacuo, the residue is dissolved in ether and then treated with 0.5 equivalent oxalic acid in ethanol solution. The resulting semi-oxalate is filtered, washed with boiling methanol-water (1:3), filtered again and dried (M.p.= 214° C.; yield: 27%).
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-3d13a2696d7346819c9049d84c7ccdfa |
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| 出典メモ | uspto-grants-1979_08 |
|---|
