Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methyl iodide → 4-([(4'-Difluoromethoxy-biphenyl-4-yl)-methyl-amino]-methyl)-5-methyl-furan-2-carboxylic acid methyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 4-(4'-Difluoromethoxy-biphenyl-4-ylaminomethyl)-5-methylfuran-2-carboxylic acid methyl ester | HCID 58824180 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 4-([(4'-Difluoromethoxy-biphenyl-4-yl)-methyl-amino]-methyl)-5-methyl-furan-2-carboxylic acid methyl ester | HCID 58824166 | 63.8% |
반응 단계
Iodomethane (91 mg, 0.64 mmoles) and potassium carbonate (88 mg, 0.64 mmoles) were added to a solution of 4-(4′-difluoromethoxy-biphenyl-4-ylaminomethyl)-5-methyl-furan-2-carboxylic acid methyl ester (170) (62 mg, 0.16 mmoles) in N,N-dimethylformamide (10 ml) and the mixture stirred at room temperature for 36 hours under an argon atmosphere. The mixture was then heated at 35° C. for 21 hours. The mixture was partitioned between dichloromethane and water, the organic phase separated and dried (MgSO4). After evaporation of the solvent, the residue was purified by flash chromatography, using cyclohexane/ethyl acetate 99:1v/v as eluent, to afford compound 175(41 mg) as a brown oil. This was used directly in part (b).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07196089B2 |
| 출처 데이터셋 | uspto-grants-2007_03 |
| ORD ID | ord-5f0ff8c15389453fbf901f9f893a5ad8 |
| 출처 메모 | uspto-grants-2007_03 |