[CH:1]1[C:6]([S:7]([C:10]2[CH:15]=[CH:14][C:13]3C(OC(=O)[C:12]=3[CH:11]=2)=O)(=[O:9])=O)=[CH:5][C:4]2C(OC(=O)[C:3]=2[CH:2]=1)=O>C1CCCCC1>[CH:13]1[CH:12]=[C:11]2[C:5]3[C:6]([S:7](=[O:9])[C:10]2=[CH:15][CH:14]=1)=[CH:1][CH:2]=[CH:3][CH:4]=3The cyclohexane extracts (containing DSDA) were combined and concentrated to an oil which was added hot (over 70° C.) in a thin stream over 5 min to a very vigorously agitated solution of 1.1 N aqueous sodium hydroxide (300 ml) at 95° C. Granules of DBTO were rapidly formed. The DBTO slurry was agitated vigorously at 90°-95° C. for 10-15 minutes, then cooled to 30° C. and filtered. The DBTO cake was thoroughly washed with water (3×100 ml) and dried (25-33% loss on drying).
Wird geladen…