関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Triethylamine hydrochloride | HCID 11130 | — |
| 反応物 | 3-(4-Propylheptyl)morpholine | HCID 11096343 | — |
| 反応物 | Glutaric acid monomethylester chloride | HCID 53445129 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 3-(4-Propyl-heptyl)-4-(5-hydroxypentyl)morpholine | HCID 14721997 | — |
反応手順
A mixture of 8.0 grams (0.035 moles) of 3-(4-propyl-heptyl)-morpholine, 4 grams of triethylamine, 5.8 grams (0.035 moles) of glutaric acid-monomethylesterchloride and 100 ml. of benzene were refluxed for 3 hours. After cooling the triethylamine hydrochloride formed was removed by filtration and the benzene solution was directly admixed with 12 grams of lithium aluminum hydride in 500 ml of ether. The reaction mixture was refluxed for 8 hours and decomposed by slow addition of water and sodium hydroxide. The precipitate was filtered off. The ether solution was dried and evaporated to dryness and the residue was distilled at 144°-146° C./ 0.01 mm Hg.; yield 9.8 grams (89%). The base obtained was dissolved in ether and the hydrochloride precipitated with hydrochloric acid in ethanol. After recrystallization from ethylacetate/ether, the melting point was 59°-60° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04894221 |
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| 出典データセット | uspto-grants-1990_01 |
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| ORD ID | ord-4c14020038ae41a6a62069f37120219d |
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| 出典メモ | uspto-grants-1990_01 |
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