참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethyl Bromide | HCID 6332 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 3',5'-Dihydroxyacetophenone | HCID 103993 | — |
| 반응물 | Cyclohexane, (bromomethyl)- | HCID 137636 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 1-(3-Cyclohexylmethoxy-5-ethoxyphenyl)ethanone | HCID 58136836 | — |
반응 단계
1-(3,5-Dihydroxyphenyl)ethanone (1.0 g) and ethyl bromide (0.531 ml) were dissolved at RT in DMF (20 ml), and sodium hydride (189 mg) was added. After stirring at 50° C. for 2 h, cyclohexylmethyl bromide (1.36 ml) was added, followed by further sodium hydride (315 mg). After stirring at 50° C. for another 2 h, the DMF was drawn off and the residue was taken up in EA, washed with water, dried, filtered and concentrated. The residue was purified using silica gel (80 g cartridge, n-heptane/EA gradient of 0-20% within 60 min). 378 mg of the title compound were obtained. LC-MS rt: 2.07 min [M+H]+: 277.2 (met. a)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08198272B2 |
|---|
| 출처 데이터셋 | uspto-grants-2012_06 |
|---|
| ORD ID | ord-441edbb569074703bb411e949a19166b |
|---|
| 출처 메모 | uspto-grants-2012_06 |
|---|