Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methyl iodide → Methyl-4-(5-iodoindazole-1-yl)-benzoate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 4-(5-Iodoindazole-1-yl)-benzoic acid | HCID 59339745 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | Methyl-4-(5-iodoindazole-1-yl)-benzoate | HCID 66812731 | 76.8% |
반응 단계
K2CO3 (7.35 g, 53.2 mmol) is suspended in 110 mL DMF. 4-(5-iodoindazole-1-yl)-benzoic acid (17.6 g, 48.33 mmol), dissolved in 25 mL DMF, is added dropwise. The reaction mixture is stirred for 30 min at r.t. Subsequently CH3I (3.31 mL, 53.2 mmol) is added dropwise (temperature rises to 30° C.). The reaction mixture is stirred overnight at r.t. and then poured on ice water. It is three times extracted with ethyl acetate. The combined organic extracts are washed twice with water and brine. After drying over Na2SO4 and filtration the solvent is evaporated. The residue is purified by chromatography (silicagel, eluents: ethyl acetate/hexane) yielding 14.03 g (76.8%) of the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07728030B2 |
| 출처 데이터셋 | uspto-grants-2010_06 |
| ORD ID | ord-4339b0ab9d0b40d582cb4138a77dda1e |
| 출처 메모 | uspto-grants-2010_06 |