Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triphenylphosphine → Methyl 4-bromo-5-methylfuran-2-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | Methyl 4,5-Dibromo-2-furancarboxylate | HCID 4135083 | — |
| 반응물 | HCID 178477798 | HCID 178477798 | — |
| 촉매 | Palladium Chloride | HCID 24290 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | Methyl 4-bromo-5-methylfuran-2-carboxylate | HCID 604544 | 1,830.4% |
반응 단계
To a mixture of the compound (1.80 g) obtained in Example 128a, palladium chloride(II) (0.02 g), triphenylphosphine (0.07 g) and tetrahydrofuran (30 mL) was added MeZnCl (2M tetrahydrofuran solution, 9.5 ml), and the mixture was heated under reflux for 4 hr under a nitrogen atmosphere. The reaction mixture was cooled to room temperature, saturated aqueous ammonium chloride was added, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was purified by column chromatography (carrier: silica gel, eluent: hexane ethyl acetate) to give the title compound (1.07 g) as a colorless solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08461348B2 |
| 출처 데이터셋 | uspto-grants-2013_06 |
| ORD ID | ord-5f3bca02527d470a924e211a0b5035a5 |
| 출처 메모 | uspto-grants-2013_06 |