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Hydrochloric Acid → 1,3-Dinaphthyl-1,3-propanedione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | 1-Acetylnaphthalene | HCID 13663 | — |
| 反応物 | Sodium amide | HCID 24533 | — |
| 反応物 | Methyl 2-naphthoate | HCID 137605 | — |
| 生成物 | 1,3-Dinaphthyl-1,3-propanedione | HCID 15259366 | — |
反応手順
4.75 gr of 50% slurry of sodium amide was suspended in 150 ml of anhydrous ether in a 250 ml round bottom flask that was equipped with a magnetic stir bar and a condenser. To this suspension was added 5.1 gr of solid acetonaphthone and continued stirring for 5 min at room temperature. After 5 minutes, 5.58 gr of methyl-2-naphthoate was added in one lot. At this point, the reaction flask was transferred to an oil bath and the bath temperature was raised so that the contents reflux gently in ether for 3 hours. The contents were then poured onto 300 gr of solid ice. On acidification with conc. HCl, solid product fell out of solution. The solid product was filtered and recrystallized in ether/methanol mixture.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07053249B2 |
| 出典データセット | uspto-grants-2006_05 |
| ORD ID | ord-9f0f95347bfe4bd7a6d3c92cbae0449e |
| 出典メモ | uspto-grants-2006_05 |