참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Hydroxide | HCID 14797 | — |
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | N-(1-Cyanocyclopentyl)pentanamide | HCID 11790092 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 2-Butyl-1,3-diazaspiro(4.4)non-1-en-4-one hydrochloride | HCID 10176995 | 60.8% |
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
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06211382B1 |
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| 출처 데이터셋 | uspto-grants-2001_04 |
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| ORD ID | ord-ecc3c624db6a4d6dbb7559dbd80c9c89 |
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| 출처 메모 | uspto-grants-2001_04 |
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