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HRID 974597作成日:2026年10月24日

Piperidine → 1-[3-[3-(Trifluoromethyl)phenoxy]-1-azetidinylcarbonyl]piperidine

https://huagongshe.com/ja/reaction/974597

反応式

関与物質

役割名称HCID仕込み量
反応物PiperidineHCID 8082—
反応物Potassium CarbonateHCID 11430—
反応物1-Chlorocarbonyl-3-[3-(trifluoromethyl)phenoxy]azetidineHCID 19799606—
溶媒BenzeneHCID 241—
溶媒TetrahydrofuranHCID 8028—
生成物1-[3-[3-(Trifluoromethyl)phenoxy]-1-azetidinylcarbonyl]piperidineHCID 15053390—

反応条件

温度-70 °C

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

DOI10.6084/m9.figshare.5104873.v1
特許番号US05068231
出典データセットuspto-grants-1991_11
ORD IDord-7b1896573f7d4ba6a0a5bb624f7954e5
出典メモuspto-grants-1991_11