Downstream synthetic route of 5317-33-9

As the paragraph descriping shows that 5317-33-9 is playing an increasingly important role.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.5317-33-9,3-(4-Methylpiperazin-1-yl)propan-1-ol,as a common compound, the synthetic route is as follows.,5317-33-9

g) is thereby obtained in the form of cream-coloured crystals, m.p. 240 C. N-[3-(4-Methyl-1-piperazinyl)propoxy]phthalimide may be obtained in the following manner: a solution of 1-(3-hydroxypropyl)-4-methylpiperazine (8.4 g), N-hydroxyphthalimide (8.2 g) and triphenylphosphine (13.1 g) in tetrahydrofuran (120 cc) is cooled to a temperature in the region of 0 C. and ethyl azodicarboxylate (10.1 g) is added in the course of 30 minutes. The solution obtained is stirred at a temperature in the region of 20 C. for 18 hours and is then concentrated to dryness under reduced pressure (20 mm Hg; 2.7 kPa) at a temperature in the region of 60 C. The crude oil obtained is chromatographed on a column 5 cm in diameter containing silica (0.063-0.2 mm) (400 g). The column is eluted with mixtures of ethyl acetate and methanol, collecting 500-cc fractions. The first 5 fractions originating from elution with pure ethyl acetate and the next 5 fractions originating from elution with a mixture of ethyl acetate and methanol (70:30 by volume) are discarded. The next fraction originating from elution with a mixture of ethyl acetate and methanol (70:30 by volume), the next 5 fractions originating from elution with a mixture of ethyl acetate and methanol (50:50 by volume) and the next 2 fractions originating from elution with pure methanol are combined and concentrated to dryness under reduced pressure (20 mm Hg; 2.7 kPa) at a temperature in the region of 60 C. N-[3-(4-Methyl-1-piperazinyl)propoxy]phthalimide (11.4 g) is thereby obtained in the form of a red oil (Rf=0.2; thin-layer chromatography on silica, eluent: ethyl acetate/methanol, 50:50 by volume).

As the paragraph descriping shows that 5317-33-9 is playing an increasingly important role.

Reference£º
Patent; Rhone-Poulenc Sante; US5086051; (1992); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics