反応 #506099

ord-ffb1b0cb7d7d4690a8f7811c56090269

反応条件

温度
100°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    洗浄wash with brine 4× (30 ml)
  2. 2
    その他dry
  3. 3
    濃縮concentrate

実験手順

Dissolve sodium methoxide (0.99 g, 18.4 mmol) in DMSO (37 ml) add methyl acetate (1 ml), add [2-(3-methoxy-phenyl)-4,4-dimethyl-cyclohexylidene]-acetic acid methyl ester (5.3 g, 18 mmol). Heat at 100° C. stirring over night. Dilute with ethyl acetate (50 ml), wash with brine 4× (30 ml), dry, and concentrate to give the title compound (5.2 g 98%): 1H NMR (CDCl3) δ 7.24-7.18 (m, 1H), 6.78-6.68 (m, 3H), 3.79 (s, 3H), 3.65 (s, 2H), 3.59 (s,1H), 2.95 (s,1H), 2.15-2.07 (m, 3H), 1.55(s, 3H), 1.49-1.46 (m,1H), 0.98 (s, 6H).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08093302B2uspto-grants-2012_01