関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Cyclopentylamine | HCID 2906 | — |
| 反応物 | Ethyl-m-[N,N-di(n-hexadecyl)aminomethyl]-thiobenzimidate Dihydrochloride | HCID 12565115 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | HCID 178443033 | HCID 178443033 | 77% |
反応手順
Ethyl-m-[N,N-di(n-hexadecyl)aminomethyl]-thiobenzimidate dihydrochloride (1.074 g., 1.5 mmoles) was added to a solution of cyclopentylamine (255 mg., 3.0 mmoles), glacial acetic acid (0.3 ml., 5.3 mmoles) and chloroform (10 ml.). The mixture was held for 72 hours at room temperature. It was then diluted to 300 ml. with chloroform, washed with saturated aqueous sodium bicarbonate solution (3 × 50 ml.), washed with saturated aqueous sodium chloride solution (3 × 50 ml.), dried (Na2SO4) and filtered. The filtrate was acidified with a 10% solution of anhydrous hydrogen chloride in dioxane (5 ml.) and then evaporated in vacuo to an oil. The oil was crystallized from warm 1,2-dimethoxyethane [850 mg., 77% yield, Rf 0.30 (4:1, benzene:ethanol on silicic acid), m.p.-forms a gel at 78° C⟧
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04066696 |
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| 出典データセット | uspto-grants-1978_01 |
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| ORD ID | ord-2b435d73dd0d4310a79e2d1e52ab56e4 |
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| 出典メモ | uspto-grants-1978_01 |
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