反応 #215285

ord-adef3961dd8f4156b9d08f6095b4a7c8

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The 3-benzoyloxy-6,7-dimethoxy-9-carbethoxymethyl-1,2,3,4-tetrahydrocarbazole was prepared
  2. 2
    ろ過The crude product in ethyl acetate was filtered through alumina
  3. 3
    その他the filtrate was evaporated to dryness under reduced pressure
  4. 4
    その他the residue was recrystallized from ethyl acetate

実験手順

The 3-benzoyloxy-6,7-dimethoxy-9-carbethoxymethyl-1,2,3,4-tetrahydrocarbazole was prepared by following an alkylation procedure similar to that described in Example 11 but using 17.6 g. of 3-benzoyloxy-6,7-dimethoxy-1,2,3,4-tetrahydrocarbazole (see Example 4) and 2.14 g. of sodium hydride (56% in mineral oil) in 200 ml. of dimethylformamide, and 8.4 g. of ethyl bromoacetate. The crude product in ethyl acetate was filtered through alumina, the filtrate was evaporated to dryness under reduced pressure and the residue was recrystallized from ethyl acetate to give 3-benzoyloxy-6,7-dimethoxy-9-carbethoxymethyl-1,2,3,4-tetrahydrocarbazole, m.p. 125°-127° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04257952uspto-grants-1981_03