Preparation method of tertiary butyl 7-hydroxyhexahydrofuro-[3,2-b] pyridine-4(2H)-carboxylic ester
A technology of hydroxyhexahydrofuran and tert-butyl, which is applied in the field of preparation of tert-butyl 7-hydroxyhexahydrofuro[3,2-b]pyridine-4(2H)-carboxylate, Industrial synthesis methods and other problems, to achieve the effects of convenient operation, easy reaction, and reliable synthesis route
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Embodiment 1
[0010] Example 1: a. Compound 1 (53 g, 0.5 mol) and compound 2 (86 g, 0.5 mol) were dissolved in acetone (300 ml) and heated to 60° C. and stirred overnight. TLC showed that the raw materials disappeared completely. The solution was concentrated under reduced pressure to remove the solvent to obtain compound 3 (132 g) as a yellow solid with a yield of 95%.
[0011] b. Disperse compound 4 (12.5 g, 0.042 mol), palladium on carbon (3 g), triethylamine (6.5 mL, 0.044 mol) and di-tert-butyl carbonate (12 g, 0.046 mol) in ethanol (200 ml) , and then stirred at room temperature under hydrogen (55 psi) pressure for 4 hours. TLC showed complete disappearance of starting material. The reaction solution was filtered under reduced pressure, and the filtrate was concentrated under reduced pressure. The crude product was dissolved in ethyl acetate (200ml) and water (150ml). The organic phase was separated, washed twice with saturated brine (200 ml), dried over anhydrous sodium sulfate an...
Embodiment 2
[0022] Example 2: a. Compound 1 (53 g, 0.5 mol) and compound 2 (86 g, 0.5 mol) were dissolved in acetone (300 ml) and heated to 60°C and stirred overnight. TLC showed that the raw materials disappeared completely. The solution was concentrated under reduced pressure to remove the solvent to obtain compound 3 (132 g) as a yellow solid with a yield of 95%.
[0023]b. Disperse compound 4 (125 g, 0.42 mol), palladium on carbon (17 g), triethylamine (65 mL, 0.44 mol) and di-tert-butyl carbonate (115 g, 0.46 mol) in ethanol (1.5 L) , then stirred at room temperature under hydrogen (55 psi) pressure for 4 hours. TLC showed complete disappearance of starting material. The reaction solution was filtered under reduced pressure, and the filtrate was concentrated under reduced pressure. The crude product was dissolved in ethyl acetate (500ml) and water (250ml). The organic phase was separated, washed twice with saturated brine (200 ml), dried over anhydrous sodium sulfate and concentra...
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