Sulfuric Acid → HCID 67099505、化合物
反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:9]2([C:15]([CH:17]([C:23]([O:25][CH2:26][CH3:27])=[O:24])[C:18](OCC)=[O:19])=[O:16])[CH2:14][CH2:13][O:12][CH2:11][CH2:10]2)[CH:6]=[CH:7][CH:8]=1.OS(O)(=O)=O>>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[C:5]2[C:4]=1[C:18]([OH:19])=[C:17]([C:23]([O:25][CH2:26][CH3:27])=[O:24])[C:15](=[O:16])[C:9]12[CH2:10][CH2:11][O:12][CH2:13][CH2:14]1参加物
3
反応条件
- 温度
- 0 °C
実験手順
Diethyl 2-(4-(3-methoxyphenyl)-tetrahydro-2H-pyran-4-carbonyl)malonate (2.1 g) was added to 5 mL H2SO4 stirred at 0° C. The mixture was stirred at room temperature for 1 hour, M+1=379. The mixture was then poured into 100 g crushed ice and extracted with EtOAc (3×50 mL). The combined organic layers were washed with H2O (20 mL) and brine (20 mL), dried over anhydrous Na2SO4, and concentrated in vacuo. The crude product was purified by column chromatography eluting with 20% EtOAc/hexane to give 0.05 g of the title compound. MS (m/z)=379 (M+H)+.