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Methanol → 3-Hydroxy-2-phenethyl-5,6-dimethoxy-2,3-dihydro-1H-isoindol-1-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | 1,4-Dioxane | HCID 31275 | — |
| 反応物 | Potassium borohydride | HCID 4192641 | — |
| 反応物 | 5,6-Dimethoxy-2-(2-phenylethyl)-1H-isoindole-1,3(2H)-dione | HCID 22757553 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-Hydroxy-2-phenethyl-5,6-dimethoxy-2,3-dihydro-1H-isoindol-1-one | HCID 22757554 | 96.9% |
反応手順
Potassium borohydride (4.87 g) dissolved in distilled water (58.7 cc) is added to 4,5-dimethoxy-N-phenethyl phthalimide (28 g) suspended in a mixture (180 cc) consisting of equal volumes of dioxan and methanol. The reaction mixture is heated under reflux for 2 hours and then concentrated to a volume of 60 cc and distilled water (450 cc) is added. After cooling, the resulting precipitate is filtered off, washed three times with distilled water (total 1000 cc) and dried under reduced pressure (20 mm Hg) at 25° C. 3-Hydroxy-2-phenethyl-5,6-dimethoxy-2,3-dihydro-1H-isoindol-1-one (27.3 g), melting at 130° C., is thus obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04128650 |
| 出典データセット | uspto-grants-1978_12 |
| ORD ID | ord-8df3739a1b454da3873c39b824b653b5 |
| 出典メモ | uspto-grants-1978_12 |