3,4-Dimethoxy-β-methyl-2-propylbenzenebutanoic acid → HCID 10825371、化合物
反応式
[CH3:1][O:2][C:3]1[C:4]([CH2:18][CH2:19][CH3:20])=[C:5]([CH2:11][CH:12]([CH3:17])[CH2:13][C:14]([OH:16])=O)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]>C(Cl)Cl>[CH3:1][O:2][C:3]1[C:4]([CH2:18][CH2:19][CH3:20])=[C:5]2[C:6](=[CH:7][C:8]=1[O:9][CH3:10])[C:14](=[O:16])[CH2:13][CH:12]([CH3:17])[CH2:11]2参加物
3
実験手順
Compound 15b (7.0 g, 25 mmol) was added to 35 g of polyphosphoric ester in 100 mL of methylene chloride and refluxed for 1 h. The reaction mixture was poured onto ice, stirred, and extracted with ether. The ether was evaporated, and the residual oil was chromatographed on silica gel using ethyl acetate/hexane to give 5.63 g (21.5 mmol, 86% yield) of 16b as white crystals: 1H NMR:(ppm) 7.49 (s, 1H), 3.89 (s, 3H), 3.87 (s, 3H), 3.00-2.23 (mult, 7H), 1.50 (mult, 2H), 1.15 (d, 3H), 1.01 (t, 3H). Anal. (C16H22O3) C,H.
後処理
- temperaturerefluxed for 1 h
- addition