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Formaldehyde → 1-[Bis(hydroxymethyl)-methyl]-6,7-dimethoxy-3,4-dihydroisoquinoline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | 3,4-Dihydro-6,7-dimethoxy-1-methylisoquinoline | HCID 22652 | — |
| 溶媒 | Sodium ethoxide | HCID 2723922 | — |
| 生成物 | 1-[Bis(hydroxymethyl)-methyl]-6,7-dimethoxy-3,4-dihydroisoquinoline | HCID 13696680 | 90% |
反応手順
To a suspension of 2.5 moles of paraformaldehyde in 300 ml of methanol 1 mole (205.3 g) of 1-methyl-6,7-dimethoxy-3,4-dihydroisoquinoline and subsequently freshly prepared sodium ethylate (1 g of sodium+50 ml of ethanol) are added at room temperature, with stirring. The reaction mixture is stirred for 5 to 6 hours, whereupon it is kept at 40° to 50 C.° for half an hour. The mixture is evaporated under reduced pressure and the obtained crystalline material is recrystallized from a mixture of acetone and ether. The aimed compound is obtained with a melting point of 129° to 131 C.°
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04656179 |
| 出典データセット | uspto-grants-1987_04 |
| ORD ID | ord-3f656b5628b14d78b120d90d97df7325 |
| 出典メモ | uspto-grants-1987_04 |