関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Azetidine | HCID 10422 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-Chlorocarbonyl-3-[3-(trifluoromethyl)phenoxy]azetidine | HCID 19799606 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-(1-Azetidinylcarbonyl)-3-[3-(trifluoromethyl)phenoxy]azetidine | HCID 15053391 | — |
反応手順
A mixture of 5.6 g (0.02 mole) of 1-chlorocarbonyl-3-[3-(trifluoromethyl)phenoxy]azetidine and 3 g (0.027 mole) of potassium carbonate in 50 ml of tetrahydrofuran was treated with 1.26 g (0.022 mole) of azetidine added dropwise to the stirred mixture. After stirring for 15 min, the reaction was treated with 10 g of ice and stirred for an additional 72 hr. The tetrahydrofuran was decanted from the salt-paste and concentrated on a rotary evaporator to yield an oil, 6.3 g. This oil crystallized when cooled to -70° C. and was recrystallized from hexane yielding 5.1 g (85%) of fine white crystals, m.p. 65°-68° 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-96d193196a4a4ba0bd61ef493f5e5a65 |
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| 出典メモ | uspto-grants-1991_11 |
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