참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | Methyl 3,5-Dibromobenzoate | HCID 621923 | — |
| 반응물 | 2-[(1E)-3-methoxyprop-1-en-1-yl]-4,4,5,5-tetramethyl-1,3,2-dioxaborolane | HCID 16217443 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | Methyl 3,5-bis[(1E)-3-methoxyprop-1-en-1-yl]benzoate | HCID 57456870 | — |
반응 단계
To a solution of methyl 3,5-dibromobenzoate (1 eq.) from the previous step in DMF (0.2 M) was added 2-[(1E)-3-methoxyprop-1-en-1-yl]-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (2.1 eq.), palladium acetate (10 mol %), triphenylphosphine (30 mol %), and 2.0 M aqueous sodium carbonate solution (5 eq.). The reaction was heated to 80° C. and stirred for 3 h. After cooling to rt, the reaction was diluted with ether. The organic extract was washed with water, brine, dried over MgSO4, and concentrated in vacuo. The crude product was purified by flash column chromatography (SiO2, 20% EtOAc in Hex) to afford the title compound as an oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08076359B2 |
|---|
| 출처 데이터셋 | uspto-grants-2011_12 |
|---|
| ORD ID | ord-d53dca1151d34266a90db378e16b3d56 |
|---|
| 출처 메모 | uspto-grants-2011_12 |
|---|
