A kind of synthetic method of 4-tert-butyl-5-ethyl-6-oxyethylene-1,4-oxazepane-4,5-dicarboxylate
A technology of dicarboxylate and oxazepane, applied to 4-tert-butyl-5-ethyl-6-oxyethylene-1,4-oxazepane-4,5-dicarboxylate In the field of synthesis, it can solve the problems of lack of reports and achieve the effects of easy operation, simplified operation process and cheap raw materials
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Embodiment 1
[0014]
[0015] 200 g of compound 2 was dissolved in 1.5 liters of anhydrous tetrahydrofuran solution, 48 g of sodium hydride was added in batches under an ice bath, and after stirring for 30 minutes, 172 g of ethyl bromoacetate reagent was added dropwise, and stirred at room temperature for 30 minutes. TLC (petroleum ether: ethyl acetate volume ratio=3:1, R f = 0.5) shows that the reaction is over, the reaction solution is slowly added to a saturated ammonium chloride solution to quench the reaction, extracted with ethyl acetate, the organic layer is dried by adding anhydrous sodium sulfate, filtered, and rotary evaporated under reduced pressure to obtain a yellow oil, and the crude Product, yield: 70%.
Embodiment 2
[0017]
[0018] 200 g of compound 2 was dissolved in 1.5 liters of anhydrous dimethylformamide solution, 48 g of sodium hydride was added in batches under ice cooling, and after stirring for 30 minutes, 172 g of ethyl bromoacetate reagent was added dropwise, and stirred at room temperature for 30 minutes. TLC (petroleum ether: ethyl acetate volume ratio=3:1, R f = 0.5) shows that the reaction is over, the reaction solution is slowly added to a saturated ammonium chloride solution to quench the reaction, extracted with ethyl acetate, the organic layer is dried by adding anhydrous sodium sulfate, filtered, and rotary evaporated under reduced pressure to obtain a yellow oil, and the crude Product, yield: 95%.
[0019] Synthesis of ethyl 2-(2-(benzylamine)ethoxy)acetate hydrochloride
[0020]
[0021] Dissolve 400 g of compound 3 in 1 liter of ethyl acetate solution, slowly add 1 liter of hydrogen chloride gas / ethyl acetate (4 mol / liter) under ice bath, and stir overnight ...
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