関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Morpholine | HCID 8083 | — |
| 反応物 | 4-(4-Methylphenyl)-3-buten-2-one | HCID 107388 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | (E)-1-(4-methylphenyl)-5-(4-morpholinyl)-1-penten-3-one hydrochloride | HCID 12842152 | — |
反応手順
8 g (0.05 mole) of 4-(4-methylphenyl)-3-buten-2-one (prepared analogously to the intermediates for the foregoing examples), 2 g (a 30% excess) of paraformaldehyde and 4.35 g (0.05 mole) of morpholine are dissolved in a mixture of ethanol (60 ml) and concentrated HCl (6 ml). The mixture is heated at reflux temperature for 18 hours. The mixture is then cooled to room temperature and diluted with acetone to a volume of 250 ml. The solution is chilled overnight. It is then concentrated to a volume of about 25 ml. The residue is triturated with ethyl alcohol. The insoluble material is filtered and recrystallized from ethyl alcohol/methyl alcohol. The resultant crystals are filtered and vacuum dried overnight, yielding 3.3 g of (E)-1-(4-methylphenyl)-5-(4-morpholinyl)-1-penten-3-one hydrochloride; m.p. 188°-190° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04400380 |
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| 出典データセット | uspto-grants-1983_08 |
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| ORD ID | ord-5f831d5144b6416ea3bb99e62c3f634f |
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| 出典メモ | uspto-grants-1983_08 |
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