Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1,1'-Carbonyldiimidazole → Tert-butyl 4-(methoxy(methyl)carbamoyl)-3-methylpiperidine-1-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| 반응물 | Methanamine, N-methoxy-, hydrochloride (1:1) | HCID 81138 | — |
| 반응물 | N-Boc-3-methyl-4-piperidinecarboxylic acid | HCID 4248616 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | Tert-butyl 4-(methoxy(methyl)carbamoyl)-3-methylpiperidine-1-carboxylate | HCID 86601647 | 65% |
반응 단계
To a solution of 1-(tert-butoxycarbonyl)-3-methylpiperidine-4-carboxylic acid (3.00 g, 12.3 mmol) in CH2Cl2 (200 mL) was added di(1H-imidazol-1-yl)methanone (2.19 g, 13.6 mmol) portionwise. After the bubbling ceased (−60 minutes), N-methoxymethanamine hydrochloride (1.32 g, 13.6 mmol) was added in one portion. The mixture was allowed to stir overnight at ambient temperature, then was washed with water, 1N HCl, and saturated sodium bicarbonate. The organic layer was dried, filtered, and concentrated to give the desired product (2.29 g, 64.8% yield) as a colorless oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08022223B2 |
| 출처 데이터셋 | uspto-grants-2011_09 |
| ORD ID | ord-cdda65218f9f41c6be844e9c79cd7bd2 |
| 출처 메모 | uspto-grants-2011_09 |