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Water → 7-Methoxy-3,4-dihydroisoquinolin-1(2H)-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Methanesulfonic Acid | HCID 6395 | — |
| 反応物 | Sodium Azide | HCID 33557 | — |
| 反応物 | 6-Methoxy-1-Indanone | HCID 334036 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 7-Methoxy-3,4-dihydroisoquinolin-1(2H)-one | HCID 13521672 | 64% |
反応手順
To a mixture of 6-Methoxy-1-indanone (15 g, 92.6 mmol), sodium azide (26.7 g, 277.8 mmol), in CHCl3 was added methane sulfonic acid (60 g, 926 mmol) via addition funnel at 0° C. Reaction mixture was warm to room temperature. Stirring was continued for 3 hr, then poured into cold water. The organics were extracted with methylene chloride and washed with water, sat. NaCl and dried over Na2SO4. Organic solution was concentrated in vacuo and the residue was purified with silica gel eluting with 20% EtOAc/Hexane to give the title compound as a yellow solid (10.5 g, 63%). MS (ES) m/z 178.1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07495111B2 |
| 出典データセット | uspto-grants-2009_02 |
| ORD ID | ord-e1c83b895e6f45ee8b99170edafb19f3 |
| 出典メモ | uspto-grants-2009_02 |