4547-02-8Relevant articles and documents
Simple synthetic process of quazepam intermediate
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Paragraph 0019-0021, (2019/05/08)
The invention discloses a simple synthetic process of a quazepam intermediate. 2-aminobenzophenone, triethylamine and DCM are taken and stirred, chloroacetyl chloride is dropped until the reaction iscomplete, liquid separation, extraction and drying are carried out, underpressure distillation is carried out, tert-butyl methyl ether is added, filtered and dried to obtain a first intermediate, thefirst intermediate, aluminium trichloride and dichloromethane are taken and stirred until the reaction is complete; the reaction solution is poured into ice 3N hydrochloric acid and liquid separationis carried out; water phase DCM extraction is carried out once; organic phases are combined and dried with anhydrous sodium sulfate; filtration is carried out, a filtrate is collected, the filtrate, 30% hydrogen peroxide, TBAB and sodium sulfide nonahydrate are stirred and heated until the reaction is complete; filtration, liquid separation and extraction are carried out, and organic phases are combined; the organic phases are washed with saturated brine and dried with anhydrous sodium sulfate; underpressure distillation is carried to remove a solvent, tert-butyl methyl ether and ethyl acetateare added into residues, pulping is carried out at room temperature, and filtration is carried out; and filter cakes are collected and dried with an infrared lamp to obtain the final product with theyield being 78.7% and the purity being 99.2%. The simple synthetic process has the advantages of easily available raw materials, simple and convenient operation and high yield.
An alprazolam intermediate benzodiazepine preparation process of thione
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, (2016/10/10)
The invention relates to a preparation method of benzodiazothioketone serving as an intermediate of alprazolam. The preparation method comprises the following steps: performing a typical acylation reaction, a cyclization reaction and a vulcanization reaction on 2-amino-5-chloro-benzophenone (M2) serving as a raw material to obtain a benzodiazothioketone crude product (the HPLC (High Performance Liquid Chromatography) content is about 94 percent); and recrystallizing the crude product in a mixed solvent at the normal temperature to obtain a fine product of which the HPLC content is over 98.5 percent, wherein the melting point of the fine product is 238-242 DEG C (the melting range is below 3 DEG C). The preparation method has the advantages of small number of synthesis steps, mild process condition, easiness in controlling a refining method, high yield, high fine product content, controllable low production cost, reduction in environmental pollution, and contribution to industrialization.
Pyrazolobenzodiazepines: Part I. Synthesis and SAR of a potent class of kinase inhibitors
Liu, Jin-Jun,Daniewski, Irena,Ding, Qingjie,Higgins, Brian,Ju, Grace,Kolinsky, Kenneth,Konzelmann, Fred,Lukacs, Christine,Pizzolato, Giacomo,Rossman, Pamela,Swain, Amy,Thakkar, Kshitij,Wei, Chung-Chen,Miklowski, Dorota,Yang, Hong,Yin, Xuefeng,Wovkulich, Peter M.
scheme or table, p. 5984 - 5987 (2010/10/21)
A novel series of pyrazolobenzodiazepines 3 has been identified as potent inhibitors of cyclin-dependent kinase 2 (CDK2). Their synthesis and structure-activity relationships (SAR) are described. Representative compounds from this class reversibly inhibit CDK2 activity in vitro, and block cell cycle progression in human tumor cell lines. Further exploration has revealed that this class of compounds inhibits several kinases that play critical roles in cancer cell growth and division as well as tumor angiogenesis. Together, these properties suggest a compelling basis for their use as antitumor agents.
Reactions of 1,4-benzodiazepinic N-nitrosoamidines with tosylmethyl isocyanide: A novel synthesis of midazolam
Del Pozo, Carlos,Macias, Alberto,Alonso, Eduardo,Gonzalez, Javier
, p. 2697 - 2703 (2007/10/03)
Reaction of 1,4-benzodiazepinic N-nitrosoamidines, used as synthetic equivalents of imidoyl chlorides, with the monoanion of tosylmethyl isocyanide is described. The process gives entry to 3-(4-tosyl)imidazo[1,5-a][1,4] benzodiazepines, compounds which have not been described yet in the literature. These systems can be derivatized to the corresponding trisubstituted 1,4-benzodiazepines by alkylation or acylation of the imidazole ring. These new heterocyclic derivatives are potentially useful in the field of medicinal chemistry. In addition, midazolam 3, the anesthetic properties of which are well established, can be easily prepared in one step by desulfonylation of compound 7a.
Phosphorylation of cyclic amides
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, (2008/06/13)
Compounds of the general formula STR1 are reacted with a strong base followed by a phosphorylating agent, such as dicyclicaminophosphinic halide or bis-di-lower alkylaminophosphinic halide to produce an imine of the formula STR2 wherein R is dicyclicaminophosphinyloxy or bis-di-lower alkylaminophosphinyloxy. R represents a leaving group which will undergo nucleophilic displacement with nitrogen, oxygen, sulfur and carbon containing nucleophiles, that is, nucleophiles which have, as a reactive site, a nitrogen, oxygen, sulfur or carbon atom, such that, when the cyclic imine undergoes nucleophilic displacement, there is formed C--N, C--O, C--S and C--C bonds between the carbon atom of the cyclic imine and the nucleophilic group. The end products may be utilized as intermediates in the production of pharmaceutically valuable compounds and, in some instances, are pharmaceutically valuable compounds per se.
Reaction of Phosphorus Pentasulfide with Organolithiums. An In Situ Reagent for the Preparation of Thiolactams
Goel, O. P.,Krolls, U.
, p. 162 - 164 (2007/10/02)
Phosphorus pentasulfide reacts under mild conditions with four equivalents of n-butyllithium, methyllithium or phenyllithium giving solutions in tetrahydrofuran.The new reagents in situ convert lactams to thiolactams and show significant selectivity in the type of reactive lactams.
