Allyl bromide → Methyl 2-hydroxy-2-methylpent-4-enoate
반응식
[CH3:1][O:2][C:3](=[O:7])[C:4](=[O:6])[CH3:5].[CH2:8](Br)[CH:9]=C.[In].[CH3:13]O.Cl>>[CH3:1][O:2][C:3](=[O:7])[C:4]([OH:6])([CH3:13])[CH2:5][CH:8]=[CH2:9]참가 물질
5
실험 절차
To a stirring solution of 2-oxopropionic acid methyl ester (1.0 g, 0.903 mmol), allyl bromide (1.8 mL, 21.32 mmol) in MeOH/HCl (1:4, 10 mL), is added indium powder (1.12 g, 9.76 mmol). The mixture is stirred for 3 days at room temperature. The mixture is quenched with NaHCO3 and extracted with DCM (3×50 mL). The organic layers are washed with water (2×50 mL) and brine. The combined organic layers are dried with MgSO4 and concentrated to afford 2-hydroxy-2-methylpent-4-enoic acid methyl ester: (M+H)+=145.
후처리
- customThe mixture is quenched with NaHCO3
- extractionextracted with DCM (3×50 mL)
- washThe organic layers are washed with water (2×50 mL) and brine
- dry with materialThe combined organic layers are dried with MgSO4
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-a5d2cbd258884f67a2847b8f97d9344c
- 출처 데이터셋
- uspto-grants-2010_04
- 특허 번호
- US07700633B2
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