참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | P-Xylene | HCID 7809 | — |
| 반응물 | 4-Methylmorpholine | HCID 7972 | — |
| 반응물 | 4-Ethenylphenyl acetate | HCID 75821 | — |
| 반응물 | 3,5-Difluorobenzoyl chloride | HCID 145600 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 촉매 | 1,3-BIS(2,6-DIISOPROPYLPHENYL)imidazoLIDINIUM-CHLORIDE | HCID 18454782 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 3,5-Difluoro-4'-acetoxystilbene | HCID 68742160 | 74.4% |
반응 단계
A 25 mL round bottom flask was charged with p-xylene (10 mL), Pd(OAc)2 (11.3 mg, 0.05 mmol), 1,3-bis-(2,6-diisopropylphenyl)imidazolinium chloride (21.4 mg, 0.05 mmol), 3,5-difluorobenzoyl chloride (0.89 g, 5 mmol), 4-acetoxystyrene (0.97 g, 6 mmol), and N-methyl morpholine (0.69 g, 6 mmol). The mixture was stirred at 120° C. for 3.5 h under nitrogen atmosphere. Then it was cooled to room temperature and EtOAc was added and filtered. The filtrate was washed with brine and dried over Na2SO4. Then it was filtered and purified via flash chromatography and gave the product (1.02 g, 74%) as white solid. Data are: 1H NMR (CDCl3, 300 MHz) δ 7.51 (d, J=8.4 Hz, 2H), 7.12-6.97 (m, 6H), 6.70 (t, 1H), 2.31 (s, 3H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08841477B2 |
|---|
| 출처 데이터셋 | uspto-grants-2014_09 |
|---|
| ORD ID | ord-999fdb07a7264857b0b22f06af7d7172 |
|---|
| 출처 메모 | uspto-grants-2014_09 |
|---|
