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 | Pyrrolidine, hydrochloride (1:1) | HCID 212848 | — |
| 反応物 | 1-(2,3-Dimethylphenyl)propan-1-one | HCID 12399442 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | 2-Methyl-1-(2,3-dimethylphenyl)-3-pyrrolidino-1-propanone hydrochloride | HCID 19901200 | 64.7% |
反応手順
A mixture of 1-(2,3-dimethylphenyl)-1-propanone (11.2 g), paraformaldehyde (2.70 g), pyrrolidine-hydrochloride (9.7g), and hydrochloric acid (0.5 ml) in isopropyl alcohol (15 ml) was refluxed for 8.5 hours. The reaction mixture was evaporated in vacuo to give the residue. The residue was dissolved in water and then washed with ethyl acetate. The aqueous layer was extracted with dichloromethane and then dried over anhydrous magnesium sulfate. The mixture was filtered and then the filtrate was evaporated in vacuo to give the residue. The residue was recrystallized from CH2Cl2 - AcOEt to give 2-methyl-1-(2,3-dimethylphenyl)-3-pyrrolidino-1-propanone hydrochloride (13.1 g, Y: 64.7%) as colorless prisms, m.p. 149°-151° C. IR ν (the free base)maxneat : 1690 cm-1 ##STR323##
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05057535 |
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| 出典データセット | uspto-grants-1991_10 |
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| ORD ID | ord-c280d2d08684449bb6a22c0779f86dd4 |
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| 出典メモ | uspto-grants-1991_10 |
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