참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Phosgene | HCID 6371 | — |
| 반응물 | 1-(4-Hydroxy-2,2,6,6-tetramethylpiperidin-1-yl)ethan-1-one | HCID 14549312 | — |
| 용매 | Methyl Ethyl Ketone | HCID 6569 | — |
| 생성물 | 1-Acetyl-2,2,6,6-tetramethyl-4-chlorocarbonyloxypiperidine Hydrochloride | HCID 19768077 | 52% |
반응 단계
A solution of 19.9 grams (0.1 mol) of 1-acetyl-2,2,6,6-tetramethyl-4-hydroxypiperidine in 150 ml of dry methyl ethyl ketone is added dropwise at 0° C over a 30-minute period to asolution of 28 ml (approximately 0.4 mol) of phosgene in 150 ml of methyl ethyl ketone. The reaction mixture is stirred at 0° C for one hour,then at 20° C. for eighteen hours. Excess dissolved phosgene is flushed out into an absorption trap with a stream of nitrogen. The solid precipitate is removed by filtration, washed twice with methyl ethyl ketone and dried with suction to yield 13.7 grams (52% yield) of the titlecompound which melts at 113-114° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05051511 |
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| 출처 데이터셋 | uspto-grants-1991_09 |
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| ORD ID | ord-91eb3b4282564b5f86cbf5b06c8dace3 |
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| 출처 메모 | uspto-grants-1991_09 |
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