📜2,2'-三亚甲基二-1,3-二噁戊环置于c11H10N2O2Pd(1+)*clo4(1-),水体系中,用 氘代乙腈 用作溶剂,化学反应 2.0H,以95%的收率获得戊二醛 参考文献:Pd(II)-Catalyzed Deprotection Of Acetals And Ketals Containing Acid Sensitive Functional Groups 标题:Pd(II)-Catalyzed Deprotection Of Acetals And Ketals Containing Acid Sensitive Functional Groups 摘要:The Pincer Complex [pd(C-1,O-1,N-1-L)(Ncme)]Clo4 (L = Monoanionic Ligand Resulting From Deprotonation Of The Acetyl Group Of The Dimethyl Monoketal Of 2,6-Diacetylpyridine) Is Used For The High-Yield And Selective Catalytic Hydrolysis Of Aliphatic,Aromatic,Cyclic,And Acyclic Dimethyl-Acetals,-Ketals,And Dioxolanes,Even In The Presence Of Large Substituents. Other Protecting Groups,Such As Thp Or Tbdms,Or Very Acid-Sensitive Alcohols Were Not Affected. The Catalyst Is Easily Prepared In High Yield From Pd(Aco)(2) And 2,6-Diacetylpyridinium Perchlorate Stable To Air And Moisture,Easily And Fully Recoverable And Reusable. (C) 2013 Elsevier Ltd. All Rights Reserved. Doi:10.1016/j.Tetlet.2013.12.067
专利号:US-11987826-B2 优先权日:2020-01-21 标 题:Nitrilase mutant and application thereof in the synthesis of an anti-epileptic drug intermediate 发明人:XUE YAPING; XIONG NENG; Lv Peijin; ZHENG YUGUO 权利人:UNIV ZHEJIANG TECHNOLOGY 摘要:The present invention provides a nitrilase mutant protein with increased thermal stability and its application in the synthesis of an anti-epileptic drug intermediate, wherein the mutant is obtained by mutating one or two of the amino acids at position 151, 223 and 250 of the amino acid sequence shown in SEQ ID No. 2. the thermal stability of the nitrilase mutant AcN-T151V/C223A/C250G was increased by up to 1.73 folds. The yield of the final product was up to 95% using the recombinant Escherichia coli containing the nitrilase mutant to hydrolyze 1M 1-cyanocyclohexylacetonitrile to produce 1-cyanocyclohexyl acetic acid at 35° C. And the yield of the final product was up to 97% when hydrolyzing 1.2M 1-cyanocyclohexylacetonitrile at 35° C. The final yield was up to 80% when using the nitrilase mutants obtained by the present invention to synthesize gabapentin.
专利号:US-7241900-B2 优先权日:2002-02-12 标题 :Synthesis of indole thiazole compounds as ligands for the Ah receptor 发明人:DELUCA HECTOR F; GRZYWACZ PAWEL K; SICINSKI RAFAL R 权利人:WISCONSIN ALUMNI RES FOUND 摘要:A method of synthesizing aromatic ketone compositions of formula I comprising the step of introducing a double bond into the 5 membered ring of the 4,5-dihydro-1,3-azoles moiety of formula II is disclosed. A method of synthesizing aromatic ketone compositions of formula I comprising the step of ring synthesis of the tetrahydro-1,3-azoles of formula XI is also disclosed.
专利号:US-6844461-B2 优先权日:2001-07-30 标 题:Synthesis of A-ring synthon of 19-NOR-1α,25-dihydroxyvitamin D3 from (D)-glucose 发明人:DELUCA HECTOR F; SHIMIZU MASATO; YAMADA SACHIKO 权利人:WISCONSIN ALUMNI RES FOUND 摘要:The present invention provides a method for the synthesis of an A-ring synthon phosphine oxide used in the preparation of 19-nor vitamin D compounds, and to novel synthetic intermediates formed during the synthesis. The new method prepares the phosphine oxide from (D)-glucose.
专利号:EP-2173892-B8 优先权日:2007-07-27 标题:Process for the preparation of immobilised recombinant Penicillin Acylase biocatalyst from Achromobacter sp CCM 4824 expressed in E. coli BL21 CCM 7394 and its use for the synthesis of beta-lactam antiobiotics 发明人:DATLA ANUPAMA; RAJASEKAR VYASARAYANI WILLIAMS; KYSLIK PAVEL; BECKA STANISLAV; KRISHNAKANT ASHAR TRUPTI; YOGESH ZAMBRE SUJATA; NIKUNJ KUMAR 权利人:FERMENTA BIOTECH LTD 摘要:The present invention discloses isolation of Penicillin Acylase (PA) from Achromobacter sp CCM 4824 expressed in recombinant strain E. coli BL21 CCM 7394 bearing the recombinant plasmid pKXIP1 and processing of PA into biocatalyst useful for the industrial synthesis of antibiotics. More particularly the invention discloses a synthesis of semi-synthetic β-lactam antibiotics in the reaction mixture consisting of activated acyl-donor (D-p-hydroxyphenylglycine methyl ester or amide for Amoxicillin and Cefadroxil; D-phenylglycine methyl ester or amide for Ampicillin and Cephalexin) and nucleophile (6-APA or 7-ADCA) catalyzed by PA obtained from recombinant E. coli BL21 CCM 7394 as the biocatalyst.
专利号:US-5847116-A 优先权日:1994-12-09 标 题 :Process for the preparation of intermediates useful in the synthesis of cephalosporins 发明人:WALKER DEREK; LEE JUNNING; MARTIN CHARLES R; ZHANG HAIYAN; SOGLI LORIS; BERNASCONI ERMANNO; MENON VINOD PARAKKAL 权利人:SCHERING CORP; ANTIBIOTICOS SA 摘要:A process is described for preparing 3-exomethylene cephalosporanic acid derivatives for use in the synthesis of cephalosporin antibiotics such as ceftibuten. The process comprises electrochemical reduction of a compound of the formula (IV) ##STR1## wherein: R 3 is ##STR2## is an optional sulfoxide group; n is 2 or 3; R 1 is H and R is H or NHR 2 , where R 2 is H or a protecting group selected from C 6 H 5 CH 2 OC(O)--, C 6 H 5 C(O)-- or C 1 -C 6 alkoxy-C(O)--; or wherein R and R 1 together with the carbon atom to which they are attached comprise --C(O)--, and produces the desired 3-exomethylene compounds with low levels of the corresponding 3-methyl tautomers.
专利号:US-7615629-B2 优先权日:2002-12-31 标 题 :Methods and compositions for the tandem synthesis of two or more oligonucleotides on the same solid support 发明人:ARAR KHALIL 权利人:SIGMA ALDRICH CO 摘要:The present invention relates to novel methods and novel solid support materials for the tandem synthesis of two or more different oligonucleotides on the same solid support in one synthetic run. The methods involve novel support preparations comprised of two or more types of orthogonally protected anchor groups. Subsequent to the selective removal of the first of the respective protective groups, the first oligonucleotide is assembled on the deblocked anchor groups according to standard methods, preferably via phosphoramidite chemistry. Following the capping of said first oligonucleotide, the anchor groups blocked by a second type of protective group are selectively liberated and serve as the starting point for the assembly of a second oligonucleotide, and so forth. After completion of all the syntheses on the solid support, the oligonucleotides are released from the solid support and deprotected at the nucleobases, using standard methods. Preparations obtained using the method of this invention, generally contain two or more different oligonucleotides. Such preparations are particularly useful in applications that require pairs of oligonucleotide primers, several probes at a time, duplexed nucleic acid fragments, or other combinations of oligonucleotides that are useful in applications such as PCR, sequencing, multiplexed genotyping, cloning and RNA interference. The invention includes procedures for the preparation of the novel solid supports of the invention.
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