참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Boron trifluoride etherate | HCID 8000 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | (3-Ethyloxetan-3-yl)methyl 3-pyridinecarboxylate | HCID 19992002 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 4-Ethyl-1-(3-pyridyl)-2,6,7-trioxabicyclo[2.2.2]octane | HCID 19992020 | — |
반응 단계
Boron trifluoride etherate (1.50 ml.) was added to a stirred solution of (3-ethyl-oxetan-3-yl)methyl 3pyridinecarboxylate) (1.10 gm.) in dry dichloromethane at -70°, under a current of dry nitrogen. The stirred mixture was allowed to warm up to room temperature over a period of six hours. Triethylamine (5 ml) was added and the mixture was poured into water. The aqueous mixture was extracted with dichloromethane. The extracts were washed with water, dried over anhydrous magnesium sulphate and the solvent was removed in vacuo. The residue was purified by chromatography on alumina (Alumina Woelm TSC) eluting with 1:1 dichloromethane:hexane, saturated with ammonia. 4-Ethyl-1-(3-pyridyl)-2,6,7-trioxabicyclo[2.2.2]octane was obtained as colourless crystals (Mpt. 58°-60°, from ether, hexane).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05057504 |
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| 출처 데이터셋 | uspto-grants-1991_10 |
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| ORD ID | ord-36bfde4ec6e8429e9209b303a9086810 |
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| 출처 메모 | uspto-grants-1991_10 |
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