Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → 4-[4-(t-Butoxycarbonylamino)methyl-4-hydroxypiperidin-1-yl]pyridine 1-Oxide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | 4-chloropyridine N-oxide | HCID 70724 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | tert-butyl N-((4-hydroxypiperidin-4-yl)methyl)carbamate | HCID 10868112 | — |
| 용매 | Isoamyl Alcohol | HCID 31260 | — |
| 생성물 | 4-[4-(t-Butoxycarbonylamino)methyl-4-hydroxypiperidin-1-yl]pyridine 1-Oxide | HCID 11034658 | 36.8% |
반응 단계
To a suspension in isoamyl alcohol (35 ml) of conventionally known compounds: 4-[(t-butoxycarbonylamino)methyl]-4-hydroxypiperidine (2.00 g) and 4-chloropyridine 1-oxide (1.12 g), was added sodium hydrogencarbonate (1.75 g) and the mixture was heated under reflux for 4 hours. The reaction mixture was allowed to cool and water was added thereto. The reaction mixture was extracted with methylene chloride and the organic layer was washed with saturated sodium chloride solution and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure and the resulting residue was purified by silica gel column chromatography (eluent:methylene chloride:methanol=9:1-4:1) to obtain the title compound (1.03 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06858599B2 |
| 출처 데이터셋 | uspto-grants-2005_02 |
| ORD ID | ord-784990b1458d4facbd2c0e6fab5babbd |
| 출처 메모 | uspto-grants-2005_02 |