Sulfuric Acid → HCID 22899237、化合物
反応式
OS(O)(=O)=O.[CH3:6][C:7]([CH3:25])=[CH:8][CH2:9][C:10]1[C:20](=[O:21])[C:19]2[CH:18]=[CH:17][C:16]([O:22][CH3:23])=[CH:15][C:14]=2[C:12](=[O:13])[C:11]=1[OH:24]>>[CH3:6][C:7]1([CH3:25])[O:21][C:20]2[C:19]3[CH:18]=[CH:17][C:16]([O:22][CH3:23])=[CH:15][C:14]=3[C:12]([C:11](=[O:24])[C:10]=2[CH2:9][CH2:8]1)=[O:13]参加物
3
実験手順
Concentrated H2SO4 (25 mL) was added to compound 52 (2.454 g) at 20° C. After stirring for 20 min, the mixture was diluted with ice water (500 mL). The resulting red precipitate 54 was collected by filtration, washed with water, and dried in vacuo. It was obtained as a red powder (2.36 g, 96%): 1H NMR (CDCl3) δ7.72 (1H, d, J=8.6 Hz), 7.56 (1H, d, J=2.7 Hz), 7.12 (1H, dd, J=8.6, 2.7 Hz), 3.90 (3H,S), 2.55 (2H, t, J=6.7 Hz), 1.84 (2H, t, J=6.7 Hz), 1.46 (6H, S).
後処理
- filtrationThe resulting red precipitate 54 was collected by filtration
- washwashed with water
- customdried in vacuo