Synthetic Route of 29671-92-9, These common heterocyclic compound, 29671-92-9, name is Carbamimidic chloride hydrochloride, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
A l l three-neck round-bottom flask equipped with a mechanical stirrer, a condenser, and a thermocouple was charged with ethyl 2-(6-amino-2,3-dichlorobenzylamino)acetate of formula (3B) (20.00 g, 72.0 mmol), chloroformamidine hydrochloride (12.44 g, 108 mmol) and acetonitrile (120 ml) under argon, and the suspension was heated to 40C. Then, acetic acid (21 ml, 363 mmol) was added and the suspension was heated to reflux (90C in oil bath). After 5 hours, the compound of formula (3B) was fully consumed as checked by HPLC. The suspension was diluted with acetonitrile (60 ml), and then N,N-diisopropylethylamine (44 ml, 252 mmol) was added drop-wise over approx. 3 minutes, and the suspension was stirred for an additional 75 minutes. Then, the reaction mixture was cooled to 50C and water (150 ml) was added. Stirring at 50C was continued for 1 hour. Then, the suspension was filtered, washed with water (30 ml), ethanol (50 ml), and methyl i-butyl ether (50 ml), and dried (23C, 100 mbar, N2 bleed, 18 hours) to give 13.48 g of anagrelide as a pale beige solid (73% of theory) in 99.53% purity (HPLC, external standard)).
Statistics shows that Carbamimidic chloride hydrochloride is playing an increasingly important role. we look forward to future research findings about 29671-92-9.
Reference:
Patent; SYNTHON BV; GIELING, Reinerus Gerardus; LINDEN van der, Johannes Bastiaan; VERKERK, Pascal Renart; MEL?A, Petr; WO2014/139572; (2014); A1;,
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