[C:1]1([S:7]([O-:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Na+].S(=O)(=O)(O)O.C1(S(O)=O)C=CC=CC=1.[N:25]([C:33]([O:35][CH:36]([CH3:38])[CH3:37])=[O:34])=[N:26][C:27]([O:29][CH:30]([CH3:32])[CH3:31])=[O:28]>O>[C:1]1([S:7]([N:25]([C:33]([O:35][CH:36]([CH3:38])[CH3:37])=[O:34])[NH:26][C:27]([O:29][CH:30]([CH3:31])[CH3:32])=[O:28])(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1To one-half mole of sodium benzenesulfinate in water in a 2 liter beaker is introduced 49 g (0.5 mole) of concentrated sulfuric acid. To the resulting suspension of benzenesulfinic acid is then added 101 g (0.5 mole) of diisopropyl azodicarboxylate. The mixture is stirred and heated to 60° C. (30 minutes). The yellow color of the azo ester gradually disappears. The oily product is extracted with benzene and separated from the lower aqueous layer. Removal of the benzene by evaporation leaves a clear oil which crystallizes when introduced into an 80/20 hexane/benzene mixture. The filtered crystals are dried at 60° C.
불러오는 중…
