Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methyl iodide → [2-(6-Methoxy-indazol-1-yl)-1-methyl-ethyl]-carbamic Acid Benzyl Ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | benzyl 2-(6-hydroxy-1H-indazol-1-yl)-1-methylethylcarbamate | HCID 136338685 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | [2-(6-Methoxy-indazol-1-yl)-1-methyl-ethyl]-carbamic Acid Benzyl Ester | HCID 69752536 | 92% |
반응 단계
To a solution of the product from Step A (0.95 g, 3.19 mmol) in DMF (10 mL) was added cesium carbonate (1.26 g, 3.70 mmol) followed by iodomethane (0.23 mL, 3.70 mmol) at room temperature. After stirring for 3 h, saturated aqueous ammonium chloride (30 mL) was added and the mixture extracted with ethyl acetate (3×65 mL). The combined extracts were washed with brine (10 mL), dried (MgSO4) and evaporated to a residue which was purified by chromatography (silica, 20% ethyl acetate in hexane to 30% ethyl acetate in hexane) to give a syrup (0.63 g, 92%): MS (ES) m/z 340(M+).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06956036B1 |
| 출처 데이터셋 | uspto-grants-2005_10 |
| ORD ID | ord-dfa9faadd8ec4aa0ab13300c63c17155 |
| 출처 메모 | uspto-grants-2005_10 |