Methyl 3-methoxy-4-(2-methylallyloxy)benzoate → Methyl 4-hydroxy-3-methoxy-5-(2-methylallyl)benzoate
反応式
[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]参加物
3
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-9589f7bacc00483cb6f54bbbce7c99b6
- 出典データセット
- uspto-grants-2012_02
- 特許番号
- US08119624B2
反応ノート
読み込み中…