참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | N,N,N',N'-Tetramethylmethanediamine | HCID 5829 | — |
| 반응물 | Acetic Anhydride | HCID 7918 | — |
| 반응물 | 6-bromo-2,2-dimethyl-3,4-dihydro-2H-1-benzopyran-4-one | HCID 14755364 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 6-bromo-2,2-dimethyl-3-methylene-2,3-dihydro-4H-chromen-4-one | HCID 86724278 | 87.4% |
반응 단계
N,N,N′,N′-tetramethylmethanediamine (4.8 g, 47 mmol) was added to a solution of 6-bromo-2,2-dimethyl-2,3-dihydro-4H-chromen-4-one (3.0 g, 12 mmol) and acetic acid (0.67 ml, 12 mmol) in tetrahydrofuran (43 ml), and the mixture was stirred at 70° C. for 24 hours. To the mixture was added acetic anhydride (4.4 ml, 47 mmol), and the mixture was stirred at 70° C. for 4 hours and concentrated in vacuo. The residue was directly purified by silica gel column chromatography (hexane/ethyl acetate=20:1) to afford 6-bromo-2,2-dimethyl-3-methylene-2,3-dihydro-4H-chromen-4-one (2.8 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US09242973B2 |
|---|
| 출처 데이터셋 | uspto-grants-2016_01 |
|---|
| ORD ID | ord-3d64f1bf0ce24835970266559e585534 |
|---|
| 출처 메모 | uspto-grants-2016_01 |
|---|