1312762-44-9Relevant articles and documents
Synthetic method for compound
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Paragraph 0051-0053; 0059-0060; 0062-0063, (2019/12/25)
The invention provides a synthetic method for a compound having a structural formula represented by a formula (V) shown in the specification. The method comprises the following steps: 1) performing hydrodebenzylation on a compound having a structural formula represented by a formula (I) shown in the specification to obtain a compound having a structural formula represented by a formula (II) shownin the specification; 2) allowing a compound having a structural formula represented by a formula (III) to be in contact with the compound having the structural formula represented by the formula (II)to obtain a compound having a structural formula represented by a formula (IV) shown in the specification; and 3) allowing the compound having the structural formula represented by the formula (IV) to be in contact with an acid solution to remove t-butoxycarbonyl protection, so as to obtain the compound having the structural formula represented by the formula (V). The synthetic method provided bythe invention has the advantages of a short synthetic route, a simple process, easy availability of the raw materials, simple post-treatment, good quality and a high yield, and is suitable for industrial production of tasocitinib and an intermediate of the tasocitinib.
The protection of the nitrogen of (3R, 4R) -3 - methylamino -4 - methyl piperidine asymmetric synthesis method, relevant intermediate and a method for preparing raw materials thereof
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, (2016/10/09)
The invention relates to a preparation method of nitrogen protected (3R,4R)-3-methylamino-4-methylpiperidine (I). The method comprises the following steps: carrying out a reductive amination reaction on a compound of formula (III) and (R)-1-phenylethylamine to obtain a compound of formula (II), removing chiral prosthetic groups from the compound of formula (II), and adding a methyl group to the amino group of the compound of formula (II) in order to obtain nitrogen protected (3R,4R)-3-methylamino-4-methylpiperidine (I), wherein R in each of the formula (I), the formula (II) and the formula (III) is an amino protection group or hydrogen, and the amino protection group can be C1-4 alkoxycarbonyl, benzyloxycarbonyl or benzyl groups which can be removed through hydrolysis or hydrogenation. The asymmetric synthesis method of nitrogen protected (3R,4R)-3-methylamino-4-methylpiperidine (I) has the advantages of reasonable technology, concise route, obtaining of the required product in a high ee value manner by constructing two chiral centers through chiral induced one-step reductive amination, cheap raw materials, and no waste isomer emission, and is suitable for large-scale industrialized production.