反応 #685951

ord-53c9d3b1802d425ca29fb5e81984c91c

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出extracted with ethyl acetate
  2. 2
    洗浄The organic extracts were washed with 1 N HCl, saturated sodium bicarbonate solution, and brine
  3. 3
    乾燥dried over MgSO4
  4. 4
    濃縮concentrated

実験手順

2-Acetyl-7-methoxy-3,4-dihydro-2H-naphthalen-1-one (72.5 mg, 0.33 mmol) and 4-benzyloxyphenylhydrazine hydrochloride (90 mg, 0.36 mmol) were heated in ethanol at 70° C. for 2.5 days. The reaction was diluted with water and extracted with ethyl acetate. The organic extracts were washed with 1 N HCl, saturated sodium bicarbonate solution, and brine, dried over MgSO4, and concentrated. SiO2 chromatography with 5-20% ethyl acetate/hexanes gave 42 mg of the desired product. LC-MS (C26H24N2O2 calculated 396) m/z 397 (M+H).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07897634B2uspto-grants-2011_03