Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methyl iodide → methyl 5-chloro-2,3-dihydro-2-mehtyl-1-oxo-1H-indene-2-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | Dimethyl Carbonate | HCID 12021 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 5-Chloro-1-indanone | HCID 142599 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | methyl 5-chloro-2,3-dihydro-2-mehtyl-1-oxo-1H-indene-2-carboxylate | HCID 19384693 | — |
반응 단계
To a solution of 5-chloroindanone (10 g) and dimethyl carbonate (6.0 ml) in THF (80 ml) was added a 60% oil dispersion (5.0 g) of sodium hydride at room temperature, followed by heating at reflux for 12 hours. After cooling to room temperature, methyl iodide (5.0 ml) was added thereto, and the mixture was heated again at reflux for 12 hours. The reaction mixture was poured into ice-water and extracted with dichloromethane (300 ml×3). The extract was dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The resulting residue was subjected to chromatography on silica gel to give methyl 5-chloro-2,3-dihydro-2-mehtyl-1-oxo-1H-indene-2-carboxylate (yield, 5.3 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05451607 |
| 출처 데이터셋 | uspto-grants-1995_09 |
| ORD ID | ord-4e6f8a3052034b5c93c5d14b1b1f8695 |
| 출처 메모 | uspto-grants-1995_09 |