Synthesis method of tert-butyl-1, 7-diazaspiro [3.5] nonane-1-formate
A technology of diazaspiro and synthesis method, which is applied in the field of synthesis of tert-butyl-1,7-diazaspiro[3.5]nonane-1-carboxylate, and can solve the problems such as no suitable industrial synthesis method , to achieve the effect of reasonable reaction process design, short route and appropriate yield
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[0012] Step 1: Dissolve compound 1 (200g, 2.38mol) in ethanol (1.3 L) at 25°C, add ammonium acetate (138 g, 1.80mol), heat up to 80°C for 1 hour; add ethylmalonic acid dropwise Ester (186 g, 1.41 mol) was reacted under reflux for 4 hours. TLC (petroleum ether / ethyl acetate volume ratio = 5 / 1) showed that the reaction of compound 1 was complete. The reaction solution was concentrated under reduced pressure, and the obtained crude product was neutralized to pH = 8 by adding 1N sodium hydroxide solution, and then extracted with ethyl acetate (0.5 L x 3). The organic phase was washed with saturated brine, dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure. The crude product was purified by chromatography to obtain compound 2 (169.2 g, yield: 41%).
[0013] Step 2: Dissolve compound 2 (132 g, 0.415 mol) in tetrahydrofuran (1 L), cool to 0°C, and add lithium borohydride (13.7 g, 0.623 mol) in batches. The reaction system was stirred for 0.5 hour...
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