Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methyl chloroformate → Methyl 5-(4-chlorophenyl)-6-(2,4-dichlorophenyl)-2-(pyridin-3-ylcarbonyl)furo[2,3-b]pyridin-3-ylcarbamate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methyl chloroformate | HCID 6586 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | [3-Amino-5-(4-chlorophenyl)-6-(2,4-dichlorophenyl)furo[2,3-b]pyridin-2-yl](pyridin-3-yl)methanone | HCID 9983227 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | Methyl 5-(4-chlorophenyl)-6-(2,4-dichlorophenyl)-2-(pyridin-3-ylcarbonyl)furo[2,3-b]pyridin-3-ylcarbamate | HCID 10030526 | — |
반응 단계
A solution of 0.030 g (0.0607 mmol) of the product from Example 26 in CH2Cl2 (0.6 mL) at 0° C. was treated with methyl chloroformate (5 μL; 0.0607 mmol) followed by diisopropylethylamine (10 μL; 0.0607 mmol). After the addition, the reaction mixture was warmed to room temperature and stirred for 16 hours. The reaction was quenched with saturated NaHCO3 solution. The reaction mixture was partitioned between ethyl acetate and saturated NaHCO3 solution. The organic layer was washed twice with saturated NaHCO3 solution, brine, dried (Na2SO4), filtered, and concentrated in vacuo. Purification by MPLC (silica gel; 0% to 30% ethyl acetate:hexane gradient) gave the title compound. HPLC/MS: 551.9 (M+1), 553.9 (M+3); Rt=4.24 min.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07091216B2 |
| 출처 데이터셋 | uspto-grants-2006_08 |
| ORD ID | ord-6b854e7dc2de4f828680e0b9d210b2fe |
| 출처 메모 | uspto-grants-2006_08 |