Synthesis method of 8-oxo-5-oxa-2-diazaspiro [3.5] nonane-2-tert-butyl formate
A technology of tert-butyl formate and a synthesis method, which is applied in directions such as organic chemistry, can solve problems such as no suitable industrial synthesis method, and achieves the effects of reasonable reaction process design, convenient operation and easy reaction.
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[0012] The first step: Dissolve n-butyl lithium (6.97 mL, 17.43 mol) in tetrahydrofuran (9 L), then add compound 2 (500 g, 5.81 mol) and TMEDA (202.5 g, 1.74 mol), the reaction was stirred for one hour. Then compound 1 (1.07 Kg, 6.27 mol) previously dissolved in tetrahydrofuran (2 L) was added dropwise into the above reaction system at 0°C to 10°C, and the reaction was maintained at 0°C to 10°C for 2 hours. TLC (petroleum ether / ethyl acetate volume ratio = 3 / 1) showed that the reaction was complete. Saturated ammonium chloride aqueous solution (1.5 L) was added to the reaction system, then extracted with ethyl acetate (1.5 L x 3), the organic phase was dried over anhydrous sodium sulfate and concentrated under reduced pressure to obtain the crude product, which was purified by silica gel column (Gradient elution: petroleum ether / ethyl acetate ~ petroleum ether / ethyl acetate volume ratio = 5:1 ~ 0:1) Yellow oily compound 3 (1.13 Kg crude product) was obtained with a yield of 2...
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