참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetone | HCID 180 | — |
| 반응물 | Pyrrolidine | HCID 31268 | — |
| 반응물 | 4'-Fluoro-2'-hydroxyacetophenone | HCID 2737326 | — |
| 용매 | Benzene | HCID 241 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 7-fluoro-2,2-dimethyl-3,4-dihydro-2H-1-benzopyran-4-one | HCID 15205373 | 70.7% |
반응 단계
To 1-(4-fluoro-2-hydroxyphenyl)ethanone (5.75 g, 37.3 mmol) and propan-2-one (12 mL, 37.3 mmol) in benzene (50 mL) was added pyrrolidine (3.11 mL, 37.3 mmol) and the reaction heated at 80° C. for 3 hours. The reaction was diluted with ethyl acetate (50 mL), washed with 1N HCl (50 mL), brine (50 mL), dried over magnesium sulfate and concentrated. The residue was purified by silica gel chromatography, eluting with a gradient of 5% ethyl acetate/hexanes to 50% ethyl acetate, to provide the title compound (5.12 g, 70.7% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08569522B2 |
|---|
| 출처 데이터셋 | uspto-grants-2013_10 |
|---|
| ORD ID | ord-6d485f331b4747359a3d1a54b42eca6d |
|---|
| 출처 메모 | uspto-grants-2013_10 |
|---|