참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | tert-butyl N-(4-oxocyclohexyl)carbamate | HCID 1512535 | — |
| 반응물 | Potassium tert-butoxide | HCID 23665647 | — |
| 촉매 | Butyltriphenylphosphonium bromide | HCID 159628 | — |
| 생성물 | HCID 86629083 | HCID 86629083 | — |
반응 단계
To a mixture of potassium t-butoxide (2.05 g) and anhydrous N,N-dimethylformamide (60 ml) was added butyltriphenylphosphonium bromide (7.30 g) at room temperature. The mixture was stirred for 15 minutes and then a solution of t-butyl 4-oxocyclohexylcarbamate (1.30 g) in N,N-dimethylformamide (10 ml) was added to the mixture. The reaction mixture was stirred at room temperature overnight and then saturated aqueous ammonium chloride was added to the mixture. The mixture was extracted with toluene, and the organic layer was washed with brine, dried over sodium sulfate, and then the solvent was removed in vacuo. After diethyl ether was added to the residue, the precipitate was filtered off and then the filtrate was concentrated under reduced pressure. The residue was purified by a silica gel chromatography (eluent: gradient from 100% hexane/0% ethyl acetate to 0% hexane/100% ethyl acetate) to give 1.40 g of t-butyl (4-butylidenecyclohexyl)carbamate.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07767854B2 |
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| 출처 데이터셋 | uspto-grants-2010_08 |
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| ORD ID | ord-1fa0f1a583cb4d2886f66a95cb1ac0bd |
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| 출처 메모 | uspto-grants-2010_08 |
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