61337-88-0Relevant articles and documents
Preparation method of 1-(3-cyanopyridin-2-yl)-2-phenyl-4-methylpiperazine oxalate
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Paragraph 0020; 0023; 0024; 0025; 0026; 0027; 0028-0053, (2019/08/12)
The invention discloses a preparation method of 1-(3-cyanopyridin-2-yl)-2-phenyl-4-methylpiperazine oxalate. The preparation method comprises the following steps: (1) adding 2-chloronicotinonitrile, potassium fluoride and 1-methyl-3-phenylpiperazine into DMSO (dimethylsulfoxide), carrying out nitrogen displacement, and conducting heating for a reaction; (2) pressurizing and distilling the reactionproduct, adding ethyl acetate into the rest residues, and conducting filtering; and (3) adding methanol and oxalic acid into the filtrate, conducting stirring for crystallization, and conducting filtering to obtain the product. DMSO is used as the reaction solvent, and the reaction temperature and the ratio of the raw material usage amount are optimized, so that the reaction time for preparationof 1-(3-cyanopyridin-2-yl)-2-phenyl-4-methylpiperazine is greatly shortened, and the production period is effectively shortened; the yield of 1-(3-cyanopyridin-2-yl)-2-phenyl-4-methylpiperazine is greatly improved and the quality is controllable; and the post-treatment mode of the method is simple, the whole synthesis process is simple to operate, and the cost is low.
Improved synthesis of mirtazapine
Srinivasa Rao,Dandala,Handa,Sivakumaran,Raghava Reddyt,Naidu
, p. 399 - 402 (2008/02/07)
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Novel method for the preparation of piperazine and its derivatives
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, (2008/06/13)
A novel method for the synthesis of piperazine and its derivatives of formula 1, 1wherein R is selected from hydrogen, or a lower alkyl group having 1 to 6 carbon atoms or a phenylalkyl group the alkyl of which has 1 to 4 carbon atoms; R1 is selected from hydrogen, a methyl group, a phenyl group optionally substituted with an alkyl group having 1 to 6 carbon atoms, or a phenylalkyl group the alkyl of which has 1 to 4 carbon atoms; and R2 is selected from hydrogen, or a methyl group, or a fluoromethyl group; 2comprising the steps: a. reacting an ester of formula 11 with substituted or unsubstituted ethylenediamine of formula 7 to give 3,4-dehydropiperazine-2-one and its derivatives of formula 12, wherein R, R1, R2 are as defined above and R6 is a C1 to C4 linear or branched alkyl group; and b. reacting the 3,4-dehydro-piperazine-2-one and its derivatives of formula 12 with a reducing agent to yield the piperazine and its derivatives of formula 1.