반응 #215285

ord-adef3961dd8f4156b9d08f6095b4a7c8

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

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

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04257952uspto-grants-1981_03