- 3,6-DIAMINO-PYRIDAZIN-3-YL DERIVATIVES, PHARMACEUTICAL COMPOSITIONS CONTAINING THEM AND THEIR USES AS PRO-APOPTOTIC AGENTS
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Compounds of formula (I) wherein Het1, Het2, R1, R2 and R3 are as defined in the description. Medicaments.
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Page/Page column 60-61
(2021/02/05)
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- Industrial preparation method of 2,2-dimethyl-4-hydroxymethyl-1,3-dioxolane
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The invention discloses an industrial preparation method of 2,2-dimethyl-4-hydroxymethyl-1,3-dioxolane. The industrial preparation method of the 2,2-dimethyl-4-hydroxymethyl-1,3-dioxolane comprises the steps that (1) carboxylic acid monoglyceride is prepared by esterification reaction, specifically, glycerol and carboxylic acid are used as raw materials, and under the condition of acidic catalyst,the dehydration reaction is carried out under the condition of 90-150 DEG C for 0.5-4h to obtain the carboxylic acid monoglyceride; (2) ketal cyclization reaction is carried out, specifically, the carboxylic acid monoglyceride and acetone are controlled to perform the cyclization reaction at 20-50 DEG C for 0.5-3 h under the condition of acid catalyst reaction to obtain a cyclization intermediateproduct; and (3) hydrolysis reaction is carried out, specifically, the intermediate product obtained in the step (2) is added into an alkaline solution, the mixture reacts for 0.5-1 h at 20-50 DEG C,and the 2,2-dimethyl-4-hydroxymethyl-1,3-dioxolane is obtained. The industrial preparation method of the 2,2-dimethyl-4-hydroxymethyl-1,3-dioxolane has the characteristics of green and environment-friendly process, high selectivity of industrial reaction and high conversion rate of raw materials.
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Paragraph 0044; 0045
(2019/06/13)
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- Synthesis of glycerolipids containing simple linear acyl chains or aromatic rings and evaluation of their Mincle signaling activity
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Mincle, expressed in activated phagocytes, recognizes the lipid ligand to activate the innate immune system. We have synthesized glycerol derivatives possessing simple alkyl chains or aromatic rings and elucidated their structure-activity relationships us
- Matsumaru, Takanori,Ikeno, Risa,Shuchi, Yusuke,Iwamatsu, Toshiki,Tadokoro, Takashi,Yamasaki, Sho,Fujimoto, Yukari,Furukawa, Atsushi,Maenaka, Katsumi
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supporting information
p. 711 - 714
(2019/02/06)
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- Preparation method for emtricitabine isomer
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The invention discloses a preparation method for an embritabine isomer. The preparation method comprises the following steps: with Solketal as a starting material, allowing the Solketal to undergo a six-step reaction of esterification, hydrolysis, oxidation, condensation cyclization, acetylation and glycosylation condensation so as to synthesize four mixture intermediates of emtricitabine; and splitting the four isomer intermediates into a cis-isomer mixture and a trans-isomer mixture through a chiral reagent. According to the invention, by adoption of a simple starting material, a mixture forsplitting key intermediates of four optical isomers of the emtricitabine is synthesized through the six-step reaction, and chiral acid is utilized to split the four isomers into a mixture of cis andtrans isomers, so the preparation method provided by the invention has the advantages of simple and convenient operation, high yield and high isomer chiral purity.
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Paragraph 0068; 0069
(2019/04/26)
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- Utilization of hexabromoacetone for protection of alcohols and aldehydes and deprotection of acetals, ketals, and oximes under UV irradiation
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Hexabromoacetone (HBA) was efficiently used for the protection of alcohols and aldehydes and deprotection of benzaldehyde dimethyl acetal, solketal, and other acetals and ketals. In only 10?min, the protection of glycerol yielded 90% of solketal and protection of benzaldehyde gave 95% of benzaldehyde dimethyl acetal. The deprotection of benzaldehyde dimethyl acetal under UV irradiation gave over 90% yield of benzaldehyde within 15?s using only 2.5?mol% of HBA. HBA was also successfully used for deoximation. Solvent was found to play an important role in the efficiency of HBA for these reactions.
- Chaiseeda, Kittichai,Chantharadet, Ladawan,Chavasiri, Warinthorn
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p. 1305 - 1323
(2017/10/30)
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- ANTIBACTERIAL COMPOSITION INCLUDING BENZOIC ACID ESTER AND METHODS OF INHIBITING BACTERIAL GROWTH UTILIZING THE SAME
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Antibacterial compositions and methods for inhibiting bacterial growth are disclosed. The antibacterial compositions can include a carrier and an antibacterial agent including a benzoic acid ester. The benzoic acid ester can have a carbon chain having a length of two to ten. The benzoic acid ester can have a hydroxyl group on the carbon chain.
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Page/Page column 23
(2018/08/26)
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- Selective functionalization of the primary hydroxy group in triols
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A procedure was suggested for preparing functionally substituted 1,2-diols by O-alkylation of hydroxyalkyl-1,3-dioxacyclanes with alkyl halides, followed by acid hydrolysis. The conditions for selective cleavage of the ethers obtained were found. (2,2-Dimethyl-1,3-dioxolan-4-yl)methyl benzoate under the conditions of acid deacetalization undergoes saponification of the ester group.
- Raskil'Dina,Valiev,Sultanova,Zlotskii
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p. 1599 - 1604
(2016/02/18)
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- Transesterification catalyzed by iron(III) β-diketonate species
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A practical and clean protocol for transesterification catalyzed by a 5 mol % cheap, non-toxic and moisture stable Fe(acac)3 or other iron(III) β-diketonate species in solvent, such as heptane under azeotropic condition is developed. A remarkable rate enhancement was observed upon the addition of 5 mol % of an inorganic base, such as Na2CO3, which suggests that faster formation of a dimeric μ-alkoxy-bridged iron(III) species under alkaline conditions facilitates catalytic turnover. This system provides smooth transesterification over a wide range of structurally diverse esters and alcohols without disturbing functional groups. In addition, the use of iron β-diketonate complexes as catalysts is more environmentally friendly, safer, and economical than other transition-metal catalysts. Preliminary mechanistic studies indicate that the active catalyst is likely a dimeric μ-alkoxy-bridged iron(III) species, as determined by X-ray crystallography of [Fe(dbm)2(O-n-Bu)]2 derived from the alcoholysis of Fe(dbm)3 under alkaline conditions.
- Weng, Shiue-Shien,Ke, Chih-Shueh,Chen, Fong-Kuang,Lyu, You-Fu,Lin, Guan-Ying
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supporting information; experimental part
p. 1640 - 1648
(2011/04/17)
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- PROCESS FOR THE MANUFACTURE OF CIS(-)-LAMIVUDINE
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An improved process for the manufacture of Lamivudine. The process involves: (a) resolution of racemic lamivudine (intermediate of formula IX) to cis (±) lamivudine of formula (XII) by forming a crystalline salt and separating the product from an organic solvent by fractional crystallization; (b) resolution of cis (±) lamivudine to cis (?) isomer involving formation of S-Binol adduct of formula XIV.
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Page/Page column 10-11
(2011/10/31)
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- Synthesis of aminopropyl phosphonate nucleosides with purine and pyrimidine bases
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The synthesis and antiviral evaluation of new acyclic phosphonate nucleosides related to HPMPC (Cidofovir) has been described. These aminopropyl phosphonate nucleosides 1-3 have an amino function within either the acyclic chain (series 2 and 3) or as subs
- Zhou, Ding,Lagoja, Irene M.,Van Aerschot, Arthur,Herdewijn, Piet
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- Enhanced enantioselectivity of Bacillus coagulans in the hydrolysis of 1,2-O-isopropylidene glycerol esters by thermal knock-out of undesired enzymes
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The enantioselective hydrolysis of different (RS)-1,2-O-isopropylidene glycerol esters has been achieved with whole cells of Bacillus coagulans NCIMB 9365 furnishing the (S)-alcohol as the major enantiomer. The reaction is catalysed by a thermostable cell-bound carboxylesterase and improvement of the enantioselectivity has been achieved by heat treatment of the whole cells, which causes the knock-outs a non-enantioselective competing enzyme. Thermally-treated cells hydrolysed (RS)-1,2-O-isopropylidene glycerol esters with high enantioselectivity, the highest enantiomeric ratio (80-100) being observed for the benzoate. The biocatalyst displayed good stability and could be re-used after filtration for 12 cycles before showing significant loss of activity; repeated biotransformation batches allowed the recovery of 9.55 g/L of enantiomerically pure (S)-isopropylideneglycerol benzoate starting from 24.0 g/L of the racemic mixture.
- Romano, Diego,Falcioni, Francesco,Mora, Diego,Molinari, Francesco,Buthe, Andreas,Ansorge-Schumacher, Marion
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p. 841 - 845
(2007/10/03)
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- Process for preparation of 1,3-dioxolane-4-methanol compounds
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PCT No. PCT/JP97/03165 Sec. 371 Date Feb. 8, 1999 Sec. 102(e) Date Feb. 8, 1999 PCT Filed Sep. 9, 1997 PCT Pub. No. WO98/11087 PCT Pub. Date Mar. 19, 1998A process for preparing easily and economically a 1,3-dioxolane-4-methanol compound in a racemic form or an optically active form with high purity and in high yield. The process comprises reacting an alkali metal or alkaline earth metal salt of an alcohol or a carboxylic acid with a halogenomethyl-1,3-dioxolane which is prepared by acetalizing a halogeno-1,2-propanediol of a formula (1) wherein X is a halogen atom, in an acid catalyst to conduct esterification or etherification, and then hydrolyzing the ester group and hydrogenolyzing the ether group to prepare a 1,3-dioxolane-4-methanol compound of a formula (5) wherein R1 and R2 are hydrogen atom, alkyl having 1 to 4 carbon atoms or phenyl, and R1 and R2 may form a cycloalkyl ring having 3 to 6 carbon atoms with the adjacent carbon atoms.
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- Stereoselective Syntheses of Both Enantiomers of Ketoconazole from (R)- and (S)-Epichlorohydrin
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Stereoselective syntheses of both enantiomers of ketoconazole (1) from commercially available (R)- or (S)-epichlorohydrin has been developed.The key-step of syntheses involves the selective substitution of the methylene chlorine atom by benzoate on a mixture of (2S,4R)-14a and (2R,4R)-15a or of their enentiomers, followed by crystalization of the corresponding cis-benzoates, (2R,4R)-18 or (2S,4S)-18, from which (+)- or (-)-1 were obtained as described for (+/-)-1.The ee's of (+)- and (-)-ketocanazole were determined by HPLC on the CSP Chiracel OD-H.
- Camps, Pelayo,Farres, Xavier,Garcia, Luisa,Ginesta, Joan,Pascual, Jaume,et al.
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p. 1283 - 1294
(2007/10/03)
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- A CONVENIENT SYNTHESIS OF PROTECTED α-HYDROXYACETALDEHYDES
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Starting from 2,3-O-isopropylideneglycerol (1), a general procedure for the preparation of protected α-hydroxyacetaldehydes has been developed.
- Shiao, Min-Jen,Yang, Chia-Yu,Lee, Shi-Hung,Wu, Teh-Chun
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p. 359 - 366
(2007/10/02)
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- A STUDY ON THE SYNTHESIS OF CARUMONAM STARTING FROM AN α-AMINO ACID
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As part of a study on the synthesis of carumonam (1), a method starting from an α-amino acid was investigated.Cycloaddition of the mixed anhydride, derived from carbobenzoxyglycine (7) and isopropyl chloroformate, with the chiral imine (11b), derived from
- Hashiguchi, Shohei,Maeda, Yoshiharu,Kishimoto, Shoji,Ochiai, Michihiko
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p. 2273 - 2283
(2007/10/02)
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