반응식
[NH2:1][C:2]1[C:7]([O:8][CH2:9][CH3:10])=[CH:6][C:5]([CH2:11][OH:12])=[CH:4][C:3]=1[O:13][CH2:14][CH3:15]>CN(C=O)C.O=[Mn]=O>[NH2:1][C:2]1[C:3]([O:13][CH2:14][CH3:15])=[CH:4][C:5]([CH:11]=[O:12])=[CH:6][C:7]=1[O:8][CH2:9][CH3:10]참가 물질
4
실험 절차
To a solution of (4-amino-3,5-diethoxy-phenyl)-methanol (0.79 g, 3.74 mmol) in DMF (20 mL) was added MnO2 (1.63 g, 18.70 mmol). The reaction mixture was stirred for 24 h at rt, filtered through Hyflo, the filtrate extracted with ethyl acetate (3×50 mL) and the combined organic phases dried over MgSO4 providing 0.69 g (88%) of the title compound. 1H NMR (300 MHz, DMSO): δ1.46 (t, J=7.0 Hz, 3H), 4.15 (q, J=7.0 Hz, 2H), 4.50 (br s, 2H), 7.04 (s, 2H), 9.70 (s, 1H).
후처리
- filtrationfiltered through Hyflo
- extractionthe filtrate extracted with ethyl acetate (3×50 mL)
- dry with materialthe combined organic phases dried over MgSO4 providing 0.69 g (88%) of the title compound
출처 및 근거
- ORD 기록
- ord-906b1ab5bd6c4313ad21a37d895959eb
- 출처 데이터셋
- uspto-grants-2010_08
- 특허 번호
- US07772253B2
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