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HRID 322812생성일: 2026년 10월 25일

Potassium Hydroxide → 2-Butyl-1,3-diazaspiro(4.4)non-1-en-4-one hydrochloride

https://huagongshe.com/reaction/322812

반응식

참여 물질

역할이름HCID투입량
반응물Potassium HydroxideHCID 14797—
반응물Ammonium ChlorideHCID 25517—
반응물N-(1-Cyanocyclopentyl)pentanamideHCID 11790092—
용매MethanolHCID 887—
용매WaterHCID 962—
생성물2-Butyl-1,3-diazaspiro(4.4)non-1-en-4-one hydrochlorideHCID 1017699560.8%

반응 조건

온도55 °C

반응 단계

To 19.6 g (0.1 mol) of 1-cyano-1-n-pentanoylaminocyclopentane dissolved in 70 ml of methanol, 25 g (0,46 mol) of potassium hydroxide dissolved in 50 ml of water was added. The resulting solution was stirred and heated at 50-60° C., then under reflux conditions for 2,5 hours. The pH was decreased by the addition of 25 g of ammonium chlorid, then methanol was distilled off. The residue was extracted with 50 ml and 2×30 ml of toluene, the combined organic phases were evaporated to constant weight The residual 16 g of title compound was dissolved in 100 ml of acetone, the pH of the resulting solution was adjusted to 1-2 with hydrochloric acid solution, the mixture was crystallized, the crystals were collected by filtration to obtain 14 g of the title compound, yield 60.8%.

출처 및 근거

DOI10.6084/m9.figshare.5104873.v1
특허 번호US06211382B1
출처 데이터셋uspto-grants-2001_04
ORD IDord-ecc3c624db6a4d6dbb7559dbd80c9c89
출처 메모uspto-grants-2001_04