| 摘要 |
PURPOSE: A method of preparing 10H-dibenzo£b,f|£1,4|thiazepin-11-one is provided, thereby requiring no organic solvent, and preventing the formation of waste acid and harmful compounds by removing the activation process of carbonylic acid in cyclization reaction. CONSTITUTION: The method of preparing 10H-dibenzo£b,f|£1,4|thiazepin-11-one represented by formula (1) comprises the steps of: reacting dithiosalicylic acid of formula (2) with 1-chloride-2-nitrobenzene in basic water-soluble solution in the presence or absence of reducing agent to prepare 2-(2-nitrophenylsulfaryl) benzoic acid of formula (3); hydrogenating the 2-(2-nitrophenylsulfaryl) benzoic acid of formula (3) to prepare 2-(2-aminophenylsulfaryl) benzoic acid of formula (4) in the presence of solvent and heterogeneous metal catalyst; and direct cyclization of the 2-(2-aminophenylsulfaryl) benzoic acid of formula (4) in the presence or absence of organic solvent and acid catalyst, wherein the basic water-soluble base is sodium hydroxide, potassium hydroxide, lithium hydroxide, sodium carbonate, potassium carbonate or sodium bicarbonate; the metal catalyst is Raney-Ni, Ru, Pd, Pt or Rh; the solvent in the preparation of 2-(2-aminophenylsulfaryl) benzoic acid is water, methyl alcohol, ethyl alcohol, normal propyl alcohol or isopropyl alcohol; the acid catalyst is sulfuric acid, phosphate, nitrate, p-toluene sulfonic acid or benzene sulfonic acid; the organic solvent in the cyclization is benzene, toluene or xylene; and the reducing agent is sodium borohydride, sodium sulfate, zinc, magnesium or hydrazine.
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