Methyl 3-methoxy-4-(2-methylallyloxy)benzoate → Methyl 4-hydroxy-3-methoxy-5-(2-methylallyl)benzoate
반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:10]=[CH:11][C:12]=1[O:13]CC(C)=C)[C:6]([O:8][CH3:9])=[O:7]>CN1C(=O)CCC1>[OH:13][C:12]1[C:11]([CH2:6][C:5]([CH3:10])=[CH2:4])=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:4][C:3]=1[O:2][CH3:1]참가 물질
3
실험 절차
A solution of methyl 3-methoxy-4-(2-methylallyloxy)benzoate (130 g, 0.55 mol) in NMP (500 mL) was heated to reflux for 6 h. TLC (EtOAc/petroleum ether=1/5) showed the reaction was complete. The mixture was washed with 1 N aq. HCl and extracted with EtOAc (250 mL×3). The combined organic phases were washed with brine (400 mL), dried over Na2SO4 and concentrated to give the product (150 g, 100%) as a brown oil. The oil was used directly to the next step without further purification.
후처리
- temperatureto reflux for 6 h
- washThe mixture was washed with 1 N aq. HCl
- extractionextracted with EtOAc (250 mL×3)
- washThe combined organic phases were washed with brine (400 mL)
- dry with materialdried over Na2SO4
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-9589f7bacc00483cb6f54bbbce7c99b6
- 출처 데이터셋
- uspto-grants-2012_02
- 특허 번호
- US08119624B2
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