Preparation method of di-tert-butyl dicarbonate
A technology of di-tert-butyl ester and dicarbonic acid, applied in the field of preparation of di-tert-butyl dicarbonate, can solve the problems of unenvironmental protection, difficult purification, and high production cost, and achieve the effects of reducing waste water volume, simple process and reducing production cost.
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[0022] The preparation method of di-tert-butyl dicarbonate comprises the following steps:
[0023] (1) Synthesis of sodium tert-butoxide: add 20g sodium metal to 400g xylene, heat to 130-140°C to obtain sodium sand, slowly add 95-96g tert-butanol dropwise at this temperature to obtain sodium tert-butoxide The solution was cooled to below 5°C and suction filtered to obtain sodium tert-butoxide, and the mother liquor was applied mechanically;
[0024] (2) Dissolve the prepared sodium tert-butoxide in petroleum ether, and pass through carbon dioxide at -5 to 10°C for 3 hours to react. After the reaction is completed, a monoester sodium salt solution is obtained;
[0025] (3) Add 2g of N,N-dimethylformamide, 1g of pyridine, and 1g of triethylamine to the monoester sodium salt solution, cool down to -5~0°C, slowly add 60g of diphosgene dropwise, drop in 1.5h After the addition was completed, the temperature was raised to room temperature (25°C), and the reaction was kept for 2 hou...
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