| 摘要 |
Non-solvated crystalline 6-hydroxy-2-(4-hydroxyphenyl) -3-(4-(2-piperidino-ethoxy) benzoyl)benzo(b)thiophene (I') hydrochloride with a defined X-ray diffraction pattern obtd. with copper radiation is new. The amt of (I').HCl is /- 95 wt% and the prod is free from chlorobenzene, aluminium salts or organolithium impurities and free from odour. In an example, a mixt of 50 g (I').HCl 1,2-dichloroethane solvate in 1125 ml MeOH and 60 ml water was refluxed until complete dissolution. The hot soln was filtered and washed (200 ml MeOH). The combined filtrate was concentrated by distillation removing 1207 ml distillate. The slurry was allowed to cool to room temp and filtered work-up gave (I').HCl of m.pt. 275.6 deg C, purity 99.4% and specified X-ray diffraction pattern. |
