참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1-Butyne, 3-chloro-3-methyl- | HCID 70679 | — |
| 반응물 | Piperidin-4-ol | HCID 79341 | — |
| 촉매 | Copper | HCID 23978 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | 1-(1,1-Dimethyl-2-propynyl)-4-piperidinol | HCID 22744488 | — |
반응 단계
24 mg cuprous chloride and 15 mg copper powder were added to a mixed solution of 5 ml solution of 7.3 g 4-hydroxypiperidine in diethyl ether (5 ml) and water (2.5 ml) in a nitrogen atmosphere. The mixture was ice-cooled, and 2.5 ml solution of 2.7 ml 3-chloro-3-methyl-1-butyne in diethyl ether was added dropwise thereinto at a bulk temperature of 17 to 22° C. Then, it was stirred at room temperature overnight. Water was added thereto, and the resulting mixture was extracted with diethyl ether for 5 times. The organic layers were combined, and dried over potassium carbonate and then over potassium hydroxide, and filtered. The filtrate was concentrated at normal pressure. The resulting crystalline residues were collected by filtration by adding ethyl acetate/hexane thereto to give 2.54 g of the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06699870B2 |
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| 출처 데이터셋 | uspto-grants-2004_03 |
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| ORD ID | ord-581faf23c8854cc699a0ee6dafbf43cc |
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| 출처 메모 | uspto-grants-2004_03 |
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