Reference of 1116-77-4, These common heterocyclic compound, 1116-77-4, name is 4,4-Diethoxy-N,N-dimethyl-1-butanamine, 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.
Example-2: Preparation of Rizatriptan Benzoate:- l-(4-Hydrazinophenyl)methyl-l52:,4-triazole hydrochloride (7.0 kg.) in Cone. HCl (35.0 It.) is stirred for 30 min at 20-250C, to that water (140.0 It.) is added and stirred for another 30min at 20-250C. 4-(Dimethylamino) butanal diethylacetal (7.10 kg.) is added slowly at 20-250C and stirred for 60 min. The reaction mixture is hated to 70-750C and maintained for 60 min. After completion of reaction, cooled the mass to 3O0C, adjusted the pH to 6.0-6.5 and extracted with methylene chloride (2 x 35 It.). Aq.layer is separated and adjusted the pH to 10-11 and extracted with ethyl acetate (3 x 55 It.). Ethyl acetate is removed under vacuum and the residue is chromatographed on silica gel (55 kg.) and eluted with ethyl acetate (25 It.) followed by methanol (30 It.) to give Rizatriptan as residue. The obtained residue is dissolved in ethanol (15 It.) and pH is adjusted to 6.0- 6.5 with benzoic acid (1.8 kg.) in ethanol (3.5 It ) at 30-350C. The reaction mass is cooled to O0C and stirred for lhr. The product is centrifuged and washed with ethanol ( 3 It) to yield Rizatriptan benzoate (3.0 kg.) with purity >99.0%.
The synthetic route of 1116-77-4 has been constantly updated, and we look forward to future research findings.