Cl[C:2]1[S:3][C:4](Cl)=[C:5]2[C:11]=1[C:10](=[O:12])[C:9]1=[CH:13][S:14][CH:15]=[C:8]1[C:7](=[O:16])[NH:6]2.C([O-])=O.[NH4+].C(O)CC>[Pd].O>[CH:2]1[S:3][CH:4]=[C:5]2[C:11]=1[C:10](=[O:12])[C:9]1=[CH:13][S:14][CH:15]=[C:8]1[C:7](=[O:16])[NH:6]2A mixture of 125 g (0.411 mole) of 1,3-dichloro-4,5-dihydrodithieno[3,4-b:3',4'-e]azepine-5,9-dione, 125 g (1.982 moles) of ammonium formate, 50 g of 5% strength Pd/C, 50 g of active carbon, 3.125 l of propanol and 165 ml of water was refluxed for 3 hours, while stirring, after which 2.5 l of solvent were distilled off under about 100 mbar, while stirring. The residue was poured onto 3 l of ice water, and the resulting suspension was acidified with concentrated hydrochloric acid, while stirring. Stirring was continued for a further hour, after which the mixture was filtered under suction and the residue was added to 1.8 l of dimethylformamide. The stirred mixture was heated at 100° C. and then filtered again under suction. The residue (Pd/C and active carbon) was washed with 5 times 100 ml of hot dimethylformamide. The original dimethylformamide mother liquor was combined with the dimethylformamide used for washing, and the still warm combined solutions were poured onto 9 l of cold water, while stirring. The precipitate formed during this procedure was filtered off under suction, washed with water and dried at 50° C., in a drying oven under reduced pressure. 80.6 g (83% OF 4,5-dihydrodithieno[3,4-b:3',4'-e]azepine-5,9-dione were obtained in the form of beige crystals of melting point 268.5°-271° C.
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