Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1-Hydroxybenzotriazole → tert-Butyl cis(+/-)-4-{[(4-chloro-5-ethyl-1H-imidazol-2-yl)carbonyl]amino}-3-ethoxypiperidine-1-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 반응물 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 반응물 | 4-chloro-5-ethyl-1H-imidazole-2-carboxylic acid | HCID 67548929 | — |
| 반응물 | Tert-butyl cis(+/-)-4-amino-3-ethoxypiperidine-1-carboxylate | HCID 86648467 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | Dimethylacetamide | HCID 31374 | — |
| 생성물 | tert-Butyl cis(+/-)-4-{[(4-chloro-5-ethyl-1H-imidazol-2-yl)carbonyl]amino}-3-ethoxypiperidine-1-carboxylate | HCID 86648478 | 82.6% |
반응 단계
The same operation as in Example (106d) was performed using tert-butyl cis(±)-4-amino-3-ethoxypiperidine-1-carboxylate obtained in Example (112d) (0.74 g, 2.9 mmol), 4-chloro-5-ethyl-1H-imidazole-2-carboxylic acid (85% content, 0.61 g, 2.98 mmol), WSC hydrochloride (1.15 g, 6 mmol), HOBt (0.61 g, 4.5 mmol), DMA (15 mL) and dichloromethane (15 mL). The resulting residue was purified by silica gel column chromatography (elution solvent: ethyl acetate/hexane=1/4, 2/3, 3/2, 4/1) to obtain 0.96 g of the title compound as a colorless solid (82%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08536197B2 |
| 출처 데이터셋 | uspto-grants-2013_09 |
| ORD ID | ord-d9451d3b46864d14bbf02653ae0fb214 |
| 출처 메모 | uspto-grants-2013_09 |