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Water → Methyl 4-[(3-butyl-1-ethylthio-4-isoquinolinyl)-methyl]-benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Ethyl thiocyanate | HCID 10968 | — |
| 反応物 | Ammonium Hydroxide | HCID 14923 | — |
| 反応物 | Methyl 4-(3-oxo-2-phenyl-heptyl)-benzoate | HCID 18999079 | — |
| 溶媒 | Phosphorus oxychloride | HCID 24813 | — |
| 生成物 | Methyl 4-[(3-butyl-1-ethylthio-4-isoquinolinyl)-methyl]-benzoate | HCID 18999070 | — |
反応手順
0.4 ml of ethyl thiocyanate and 0.45 ml of stannic chloride were added to a solution of 1 g of methyl 4-(3-oxo-2-phenyl-heptyl) benzoate of Step C in 20 ml of phosphorous oxychloride and the mixture was stirred for 10 hours at reflux, then poured into ice-cooled water. The mixture was stirred for 15 minutes and alkalized with concentrated ammonium hydroxide. Extraction was carried out with ethyl acetate and the extracts were washed with water, dried and evaporated to dryness. The residue was chromatographed on silica (eluant: hexane--ethyl acetate (9-1)) to obtain 0.57 g of the desired product melting at 70° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05478938 |
| 出典データセット | uspto-grants-1995_12 |
| ORD ID | ord-64c9eeabc9384717812dd60ee6024c17 |
| 出典メモ | uspto-grants-1995_12 |