Method for preparing N-tert-butyloxycarbonylpiperazine acetic acid hydrochloride
A technology of tert-butoxycarbonyl and acetic acid hydrochloride, which is applied in the field of preparation of piperazine carboxylate hydrochloride, can solve the problems of low weight content and low product yield, and achieve high overall yield and excellent preparation process The effect of reasonable selection and low requirements for production equipment
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example 1
[0014] Synthesis of N-Boc-piperazine acetate hydrochloride
[0015] Under mechanical stirring, dissolve (1.5kg, 8.0mol) N-Boc-piperazine in a 10-liter acetonitrile (1.0L) reactor; cool down to 5-10°C with an ice bath; add 1.5Kg potassium carbonate; A solution of ethyl bromoacetate in acetonitrile (1.3Kg / 1.0L) was added dropwise, and the internal temperature was controlled below 25°C during the dropwise addition. After the dropwise addition, the reaction system was stirred at 20-25°C for 2 hours, and filtered; the filter cake was dissolved and extracted with water (5.0L) and methyl tert-butyl ether (5.0LX2 times), and the extracted organic liquid was combined with the filtered filtrate , Distilled under reduced pressure to obtain N-Boc-piperazine ethyl acetate with a purity of over 90%. directly used in the next hydrolysis reaction.
[0016] Under mechanical stirring, the resulting ethyl N-Boc-piperazine acetate was dissolved in tetrahydrofuran (5.0L) in a 10-liter reactor;...
example 2
[0018] Synthesis of N-Boc-piperazine acetate hydrochloride
[0019] Under mechanical stirring, dissolve (1.5kg, 8.0mol) N-Boc-piperazine in acetonitrile (1.0L) in a 10-liter reactor; cool down to 5-10°C with an ice bath; add 1.5Kg of potassium carbonate; A solution of ethyl bromoacetate in acetonitrile (1.3Kg / 1.0L) was slowly added dropwise, and the internal temperature was controlled below 25°C during the dropwise addition. After completion of the dropwise addition, the reaction system was stirred for 2 hours below 82°C, and filtered; the filter cake was dissolved and extracted with water (5.0 L) and methyl tert-butyl ether (5.0 L×2 times), and the extracted organic liquid was combined with the filtered filtrate. Distill under reduced pressure to obtain N-Boc-piperazine ethyl acetate with a purity of over 90%. directly used in the next hydrolysis reaction.
[0020] Under mechanical stirring, the resulting ethyl N-Boc-piperazine acetate was dissolved in tetrahydrofuran (5....
example 3
[0022] Synthesis of N-Boc-piperazine acetate hydrochloride
[0023] Under mechanical stirring, dissolve (1.5kg, 8.0mol) N-Boc-piperazine in acetonitrile (1.0L) in a 10-liter reactor; cool down to 5-10°C with an ice bath; add 1.5Kg of potassium carbonate; A solution of ethyl bromoacetate in acetonitrile (1.3Kg / 1.0L) was slowly added dropwise, and the internal temperature was controlled below 0°C during the dropwise addition. After the dropwise addition, the reaction system was stirred at 20-25°C for 2 hours, and filtered; the filter cake was dissolved and extracted with water (5.0L) and methyl tert-butyl ether (5.0LX2 times), and the extracted organic liquid was combined with the filtered filtrate , Distilled under reduced pressure to obtain N-Boc-piperazine ethyl acetate with a purity of over 90%. directly used in the next hydrolysis reaction.
[0024] Under mechanical stirring, the resulting ethyl N-Boc-piperazine acetate was dissolved in tetrahydrofuran (5.0L) in a 10-li...
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