2-(2-Bromophenoxy)-1-phenylethan-1-one → 7-Bromo-3-phenylbenzofuran
반응식
[Br:1][C:2]1[CH:17]=[CH:16][CH:15]=[CH:14][C:3]=1[O:4][CH2:5][C:6]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)=O>O>[C:8]1([C:6]2[C:14]3[CH:15]=[CH:16][CH:17]=[C:2]([Br:1])[C:3]=3[O:4][CH:5]=2)[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1참가 물질
3
반응 조건
- 온도
- 95 °C
실험 절차
A mixture of 2-(2-bromophenoxy)-1-phenyl-1-ethanone (6.31 g) and polyphosphoric acid (285 g) was stirred at 95° C. for 6 h. The resulting solution was cooled to 50° C. , poured in water (2 L), extracted with Et2O (2×1 L). The combined organic extracts were washed with water (4×500 ml) and brine, dried over MgSO4 and concentrated. The residual solid was filtered on a plug of silica gel using Et2O. Recrystallization in hot hexane yielded the title compound (4.63g; 78%).
후처리
- temperatureThe resulting solution was cooled to 50° C.
- extractionextracted with Et2O (2×1 L)
- washThe combined organic extracts were washed with water (4×500 ml) and brine
- dry with materialdried over MgSO4
- concentrationconcentrated
- filtrationThe residual solid was filtered on a plug of silica gel
- customRecrystallization in hot hexane
출처 및 근거
- ORD 기록
- ord-6cdbed8943fb48f68118e840327e7135
- 출처 데이터셋
- uspto-grants-2001_04
- 특허 번호
- US06211197B1
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