関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Piperidine | HCID 8082 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-Chlorocarbonyl-3-[3-(trifluoromethyl)phenoxy]azetidine | HCID 19799606 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-[3-[3-(Trifluoromethyl)phenoxy]-1-azetidinylcarbonyl]piperidine | HCID 15053390 | — |
反応手順
A solution of 5.6 g (0.02 mole) of 1-chlorocarbonyl-3-[3-(trifluoromethyl)phenoxy]azetidine in 50 ml of tetrahydrofuran was treated with 3 g (0.022 mole) of potassium carbonate and while stirring, 1.9 g (0.022 mole) of piperidine was added dropwise. The mixture was then treated with 10 g of ice and stirred for 2 hr. The tetrahydrofuran was decanted then concentrated on a rotary evaporator to yield an amber oil, 6.0 g. The oil was dissolved in benzene, washed with dilute acid then water, dried over magnesium sulfate and concentrated in vacuo. This oil crystallized when cooled to -70° C. and was recrystallized from hexane with charcoal treatment at 0° C. yielding pale tan crystals, 4.5 g (68.5%), m.p. 50°-52° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05068231 |
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| 出典データセット | uspto-grants-1991_11 |
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| ORD ID | ord-7b1896573f7d4ba6a0a5bb624f7954e5 |
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| 出典メモ | uspto-grants-1991_11 |
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