C([NH:4][C:5]1[CH:10]=[C:9]([NH:11][C:12](=[O:14])[CH3:13])[CH:8]=[CH:7][C:6]=1[O:15][CH2:16][CH2:17][CH3:18])(=O)C.NC1C=C(N)C=CC=1OCCC.C([O-])(=O)C.[Mg+2].C([O-])(=O)C.[BrH:40]>C(O)C>[BrH:40].[CH2:16]([O:15][C:6]1[C:5]([NH2:4])=[CH:10][C:9]([NH:11][C:12](=[O:14])[CH3:13])=[CH:8][CH:7]=1)[CH2:17][CH3:18]
208 parts of dried crude 6-n-propoxy-3-acetylamino-aniline obtained according to Example 7 of European Pat. No. 0,011,048 (containing, in addition to 190.3 parts of target product, 8.8 parts of 2,4-bis-acetylamino-1-n-propoxybenzene and 3.5 parts of 2,4-diamino-1-n-propoxybenzene, as well as small amounts of magnesium acetate and oxidative decomposition products) are dissolved in 300 parts of ethanol at 50° C., with stirring, and, after the solution has been cooled to 25° C., 170 parts of 48% strength hydrobromic acid are added dropwise in the course of 1.5 hours. The precipitate which has separated out is filtered off with suction at 0°-5° C., washed with two portions of 60 parts of ethanol and dried in vacuo. 257.1 parts of 6-n-propoxy-3-acetylamino-aniline hydrobromide (no impurities detectable by HPLC, purity by diazotization: 99.4%) are obtained, which corresponds to a yield of 88.9% of theory (based on the crude feed product) or 97.2% of theory (based on the target product contained therein).
Wird geladen…
