111991-20-9Relevant articles and documents
A method for preparing 2, 4, 5 - trifluorobenzene acetic acid (by machine translation)
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, (2018/12/03)
The invention discloses a 2, 4, 5 - trifluorobenzene acetic acid. The method includes the steps of: (1) the structure shown as formula A 2, 4, 5 - trifluorobenzene diazonium salt with the structure shown in formula II substituted ethylene to carry out coupling reaction, to obtain the intermediate; and (2) the intermediate through hydrolysis or oxidation of the structure is shown as formula I shown in 2, 4, 5 - trifluorobenzene acetic acid; the intermediate comprises a structure of formula IV or a compound represented by the structure of formula C shown 2, 4, 5 - trifluoro phenylacetaldehydes. (by machine translation)
A west he row sandbank and its salt synthesis method (by machine translation)
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Paragraph 0072; 0073, (2017/08/04)
The invention discloses a west he row sandbank and its salt synthesis method, in order to 2, 4, 5 - trifluorobenzene acetic acid as the starting material, through esterification, reduction, oxidation and Witting reaction, to obtain 4 - (2, 4, 5 - trifluorophenyl) - 2 - butene ethyl ester, or passes through the reduction, oxidation and Witting reaction after, to obtain 4 - (2, 4, 5 - trifluorophenyl) - 2 - butene ethyl ester. Then in BuLi or six methyl two silicon and nitrogen under the action of the alkane-sodium, with chiral amine on the hydroamination reaction, framed asymmetric amination product, through ester, condensation, hydrogenated three-step reaction to obtain sitagliptin. The west he of the spit of fland synthesis method of raw materials are cheap and easy to obtain, steps are less, the operation is easy, can be effectively reduced. The method can be the high purity of the sitagliptin, the salt of the phosphoric acid obtained after HPLC purity and sitagliptin ee values are in 99% or more, can be applied to the medical field. (by machine translation)
A method for synthesizing row sandbank west he
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, (2017/04/13)
The invention discloses a synthetic method for sitagliptin. The method comprises the following steps that: 2,4,5-trifluorobenzaldehyde is used as a starting raw material and undergoes the Wittig reaction and hydrolysis with hydrochloric acid so as to obtain 2-(2,4,5-trifluorophenyl)acetaldehyde; 2-(2,4,5-trifluorophenyl)acetaldehyde and (R)-(+)-t-butyl sulfenamide are subjected to condensation so as to obtain corresponding acetal; acetal and ethyl bromoacetate undergo the Reformatsky reaction, and then an obtained product undergoes hydrolysis so as to obtain organic acid; the organic acid and 3-(trifluoromethyl)-5,6,7,8-tetrahydro-[1,2,4]triazolo[4,3-a]pyrazine hydrochloride are subjected to condensation so as to obtain acetal of t-butyl sulfenamide of sitagliptin; and finally methanol hydrochloride is used for deprotection so as to obtain sitagliptin. The invention has the following advantages: yield in each step is high, operation is simple, reagents used in the method are conventional reagents, usage of an expensive chiral catalyst is avoided, and good industrial prospect is obtained.