[C:1]([NH:5][NH2:6])([CH3:4])([CH3:3])[CH3:2].[N:7]([C:16]([N:20]=[C:21]=[O:22])([CH2:18][CH3:19])[CH3:17])=[N:8][C:9]([N:13]=[C:14]=[O:15])([CH2:11][CH3:12])[CH3:10]>CCCCC>[N:7]([C:16]([NH:20][C:21]([NH:6][NH:5][C:1]([CH3:4])([CH3:3])[CH3:2])=[O:22])([CH2:18][CH3:19])[CH3:17])=[N:8][C:9]([NH:13][C:14]([NH:6][NH:5][C:1]([CH3:4])([CH3:3])[CH3:2])=[O:15])([CH2:11][CH3:12])[CH3:10]To a stirred solution of 5.8 grams (0.05 moles) of 76% t-butylhydrazine in 30 ml pentane in a 50 ml erlenmeyer flask cooled in a water bath was added 5.6 grams (0.025 moles) of 2,2'-azobis(2-isocyanatobutane) (from Example XXXVI) dropwise over 20 minutes while holding the reaction temperature below 30° C. After the addition was complete, the reaction was stirred for an additional 60 minutes at room temperature and filtered. The filter cake was washed with pentane and dried. The dry white solid weighed 3.3 grams (33% crude yield) and melted at 155°-160° C. with decomposition. The product had a broad strong carbonyl band at 1625- 1675 cm-1 and a broad strong NH band at 3300- 3450 cm-1 in its infrared spectrum and the isocyanate band at 2200 cm-1 was absent.
読み込み中…