Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Chloroform → HCID 67973500, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Chloroform | HCID 6212 | — |
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | Thiophene, 2,3,5-tribromo- | HCID 76592 | — |
| 반응물 | (4-Methoxyphenyl)boronic acid | HCID 201262 | — |
| 촉매 | HCID 178418397 | HCID 178418397 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 용매 | Oxolane--water (1/1) | HCID 21881883 | — |
| 생성물 | HCID 67973500 | HCID 67973500 | 65% |
반응 단계
2,3,5-Tribromothiophene (6.42 g, 20 mmol), 4-methoxyphenylboronic acid (6.38 g, 42 mmol) and sodium carbonate (8.5 g, 80 mmol) were stirred in THF/water mixture (125/50 ml) for 90 min at RT under argon flushing. Pd(PPh3)4 (693 mg, 0.6 mmol) was added. The mixture was refluxed for 16 h (TLC), cooled to RT and THF was removed by evaporation. Water was added and aqueous fractions extracted with EtOAc. The organic fractions were combined, solvent removed and the crude product purified by flash chromatography (Silica gel; hexane/chloroform/EtOAc; gradient up to 20% chloroform then 20% EtOAc) to yield 3-bromo-2,5-bis(4-methoxyphenyl)thiophene (4.9 g, 13 mmol, 65%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09176357B2 |
| 출처 데이터셋 | uspto-grants-2015_11 |
| ORD ID | ord-4ad2ec4d58e54e07bd01dbcc2fa5da29 |
| 출처 메모 | uspto-grants-2015_11 |