참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | 4-Methylmorpholine | HCID 7972 | — |
| 반응물 | Benzyl succinimido carbonate | HCID 83172 | — |
| 반응물 | 4-Bromopiperidine Hydrobromide | HCID 2734676 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | Benzyl 4-bromotetrahydro-1(2H)-pyridinecarboxylate | HCID 2776275 | 98.4% |
반응 단계
To a solution of 4-bromopiperidine hydrobromide (3.0 g, 12.2 mmol) in tetrahydrofuran (30 ml) were added 1-{[(benzyloxy)carbonyl]oxy}-2,5-pyrrolidinedione (3.20 g, 12.9 mmol), N-methylmorpholine (1.62 ml, 14.7 mmol) and 4-N,N-dimethylaminopyridine (30 mg) at room temperature, and stirred at room temperature for 16 hours. The reaction solution was poured into water and extracted with ethyl acetate. The organic layer was washed with a 1N-aqueous hydrochloric acid solution, dried over anhydrous magnesium sulfate and distilled under reduced pressure to remove the solvent, and the resulting residue was purified by a silica gel column chromatography (eluent: hexane/ethyl acetate=1/1) to obtain benzyl 4-bromo-1-piperidinecarboxylate (3.58 g, 98%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07199147B2 |
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| 출처 데이터셋 | uspto-grants-2007_04 |
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| ORD ID | ord-8ffc2216144248a1b5320f2e36839be0 |
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| 출처 메모 | uspto-grants-2007_04 |
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