Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Acetic Acid → 1,1-Dimethylethyl 4-[[4-(4-chlorophenoxy)phenyl]amino]-1-piperidinecarboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | 4-(4-Chlorophenoxy)aniline | HCID 7578 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | tert-Butyl 4-oxopiperidine-1-carboxylate | HCID 735900 | — |
| 반응물 | Sodium triacetoxyborohydride | HCID 5049666 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 1,1-Dimethylethyl 4-[[4-(4-chlorophenoxy)phenyl]amino]-1-piperidinecarboxylate | HCID 68489597 | 71.7% |
반응 단계
In a similar manner as described above in Paragraph A, a solution of 1,1-dimethylethyl 4-oxo-1-piperidinecarboxylate (1 g, 4.5 mmol) and 4-(4-chlorophenoxy)aniline (1 g, 5 mmol) in dichloromethane was stirred as acetic acid (0.39 g, 6.5 mmol) was added. After 15 minutes, sodium triacetoxyborohydride (2 g, 9.4 mmol) was added and the reaction was stirred for 3 days. The reaction was treated with aqueous sodium bicarbonate. The organic layer was washed with water, dried, and concentrated. Purification by flash chromatography on silica gel using a gradient of ethyl acetate in hexane gave 1.3 g of 1,1-dimethylethyl 4-[[4-(4-chlorophenoxy)phenyl]amino]-1-piperidinecarboxylate.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07737145B2 |
| 출처 데이터셋 | uspto-grants-2010_06 |
| ORD ID | ord-6cede7551ac24d66b323405d86425165 |
| 출처 메모 | uspto-grants-2010_06 |