Tert-butylhexahydro-2H-pyrrole[1,4]oxazepine-7(3H)-carboxylic ester preparation method
A technology of oxazepane and carboxylate, which is applied in the field of preparation of tert-butylhexahydro-2H-pyrrole[1,4]oxazepane-7(3H)-carboxylate, It can solve the problems of no suitable industrial synthesis method, etc., and achieve the effects of short synthesis route, easy reaction and convenient operation.
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[0010] Example 1: a, compound 1 (500 g, 2.95 mol) and N-benzyl hydroxylamine (659 g, 4.1 mol), potassium acetate (434 g, 4.43 mol), paraformaldehyde (500 g, 5.0 mol) Dissolve in ethanol (5 L), heat the mixture to reflux, react for 24 hours, TLC (petroleum ether / ethyl acetate volume ratio=10 / 1) shows that the reaction is complete. The reaction system was cooled to room temperature, 3L of water was added, and the reaction solution was adjusted to pH=11 with solid sodium carbonate, then extracted with ethyl acetate, the organic phase was dried with anhydrous sodium sulfate, and distilled under reduced pressure to obtain the crude compound 2 in brown oil (1 kg).
[0011] b. Dissolve compound 2 (180 g, 0.56 mol) in methanol (2 L), then add Raney nickel (100 g, 3.7 mol) into the system, control the reaction temperature at room temperature, and react at a pressure of 15 psi for 2 hours. TLC (petroleum ether / ethyl acetate volume ratio=1 / 1) showed that the reaction was complete. The ...
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