Method for synthesizing tert-butyl 6-oxo-8-oxa-2, 5-diazaspiro[3.5]nonane-2-carboxylate
A technology of tert-butyl formate and diazaspiro, applied in the field of synthesis of 6-oxylidene-8-oxa-2,5-diazaspiro[3.5]nonane-2-carboxylate tert-butyl , can solve the problems of no suitable industrial synthesis methods, etc., and achieve the effects of reasonable reaction process design, easy reaction and convenient operation
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[0012] Step 1: Dissolve compound 1 (45 g, 0.22 mol) in N,N-dimethylformamide (500 mL), add paraformaldehyde (60.2 g, 0.66 mol), and cool down to 0°C , tetrabutylammonium fluoride (5.8 g, 0.02 mol) was added to the reaction solution. The reaction was kept at 0°C for 30 minutes, then warmed to room temperature and reacted for 15 hours and 30 minutes. TLC showed the reaction was complete. The reaction was filtered with diatomaceous earth, the filtrate was poured into water and extracted with ethyl acetate, and the organic phase was dried with anhydrous sodium sulfate to obtain a white solid compound 2 (47 g, 90% purity). Yield: 90%.
[0013] 1 (400 M; CDCl 3 )
[0014] δ4.43-4.40 (d, J = 10 Hz, 2 H), 4.20-4.18 (d, J = 9.2 Hz, 2 H), 4.15-4.12(d, J = 10 Hz, 2 H), ,1.46 (s, 9 H).
[0015] The second step: Compound 2 (200 g, 0.86 mol) was dissolved in acetone (1.5L), and cesium carbonate (561 g, 1.72 mol) and ethyl bromoacetate (172 g, 1.03 mol) were added successively at r...
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