[CH2:1]=O.[ClH:3].[CH3:4][NH:5][CH3:6].[Br:7][C:8]1[CH:9]=[C:10]2[C:18](=[CH:19][CH:20]=1)[N:17]([CH3:21])[C:16]1[CH2:15][CH2:14][CH2:13][C:12](=[O:22])[C:11]2=1.O>C(O)(=O)C>[ClH:3].[Br:7][C:8]1[CH:9]=[C:10]2[C:18](=[CH:19][CH:20]=1)[N:17]([CH3:21])[C:16]1[CH2:15][CH2:14][CH:13]([CH2:4][N:5]([CH3:1])[CH3:6])[C:12](=[O:22])[C:11]2=1Paraformaldehyde (1.5 g) and dimethylamine hydrochloride (3.75 g) were added to a solution of the product of Stage (iii) (10 g) in acetic acid (70 ml) and then heated to reflux for 8 h. On cooling to ambient temperature the reaction mixture was poured into water (400 ml). The oil which separated out was triturated with ether (500 ml) to give a solid (9 g) which was partitioned between ethyl acetate (2×30 ml) and saturated aqueous sodium carbonate (100 ml). The organic phase was evaporated and the residue purified by flash chromatography (G) to give the pure free base as a solid (0.40 g). A sample (0.4 g) was dissolved in ethanol (10 ml), filtered, and ethereal HCl (6 ml) was added. On addition of dry ether (20 ml), the title compound crystallized as a solid (0.38 g) m.p. 219°-220°.
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