- METHOD FOR EXTRACTING ASYMMETRIC B-DIKETONE COMPOUND FROM B-DIKETONE COMPOUND
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The present invention provides a method of extracting an asymmetric β-diketone compound from a β-diketone compound containing at least one symmetric β-diketone compound mixed in the asymmetric β-diketone compound, and the method includes the step (A) of adjusting a pH of a mixed solution of the β-diketone compound and water at 11.5 or more and dissolving the β-diketone compound into water to form a β-diketone compound solution and the step (B) of subsequently adjusting the pH of the β-diketone compound solution at 9.5 or less and recovering the asymmetric β-diketone compound of Chemical Formula 1 separated from the β-diketone compound solution. The present invention further includes at least either (a) a step of setting the upper limit of the pH of the mixed solution to 12.5 to form a β-diketone compound solution in the step (A) and bringing the β-diketone compound solution into contact with a hydrophobic solvent or (b) a step of setting the lower limit of the pH of the β-diketone compound solution to 8.0 in the step (B).
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Paragraph 0074-0076
(2015/11/16)
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- AZAINDAZOLES
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Herein are disclosed azaindazoles of formula (I), (I), where the various groups are defined herein, and which are useful for treating cancer.
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Page/Page column 55
(2013/03/28)
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- ENHANCER OF ZESTE HOMOLOG 2 INHIBITORS
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This invention relates to novel substituted benzamide according to Formula (I) which are inhibitors of Enhancer of Zeste Homolog 2 (EZH2), to pharmaceutical compositions containing them, to processes for their preparation, and to their use in therapy for the treatment of cancers.
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Page/Page column 48
(2013/12/03)
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- Porphyrins with exocyclic rings. Part 22: Synthesis of deoxophylloerythroetioporphyrin (DPEP), three ring homologues, and five related nonpolar bacteriopetroporphyrins using a western ring closure and an improved b-bilene methodology
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Dipyrrolic intermediates incorporating five-membered carbocyclic rings are easily prepared from cyclopenta[b]pyrroles, and this unit represents the southern half of the DPEP-type geoporphyrins found in organic-rich sediments such as oil shales and petroleum. Related dipyrroles with six-, seven- or eight-membered carbocyclic rings were shown to give b-bilenes when reacted with dipyrrylmethane carbaldehydes under mildly acidic conditions. Following deprotection of the terminal ester groups, cyclization with TFA-CH(OMe)3 gave a series of ring homologues of deoxophylloerythroetioporphyrin (DPEP). The b-bilenes generated from the five-membered ring dipyrroles proved to be rather unstable and had to be used directly without purification. Cyclization gave DPEP contaminated with an etioporphyrin by-product, but these could be separated as the nickel(II) derivatives by flash chromatography. This approach gave superior yields of DPEP compared to previously reported methods. In addition, the methodology could be extended to the synthesis of related petroporphyrins, and a series of five molecular fossils derived from bacteriochlorophylls d were synthesized by this approach.
- Lash, Timothy D.,Li, Wei,Quizon-Colquitt, Desiree M.
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p. 12324 - 12342
(2008/03/13)
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- Method for preparing chiral diphosphines
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The invention concerns a method for preparing a compound of formula (1) wherein: A represents naphthyl or phenyl optionally substituted; and Ar1, Ar2independently represent a saturated or aromatic carbocyclic group, optionally substituted.
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- New insights into the reduction of β,δ-diketo-sulfoxides
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New developments in the reduction of β,δ-diketo-sulfoxides, a reaction that affords important key intermediates for total synthesis, are described. We showed without ambiguity using NMR experiments, that the β-carbonyl group is totally enolised. This result is inconsistent with the previous hypothesis, which supposed the other tautomer (enolisation at the δ-position) as the major one. We propose a rationale to explain the side reactions occurring during the reduction of unprotected β,δ-diketo-sulfoxides and showed that judicious protection of the δ-carbonyl group gave all diastereoisomers of β-hydroxy-δ-ketosulfoxides.
- Hanquet, Gilles,Salom-Roig, Xavier J.,Gressot-Kempf, Laurence,Lanners, Steve,Solladie, Guy
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p. 1291 - 1301
(2007/10/03)
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- Asymmetric hydrogenation method of a ketonic compound and derivative
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The present invention relates to a process for the asymmetric hydrogenation of a ketonic compound and derivative. The invention relates to the use of optically active metal complexes as catalysts for the asymmetric hydrogenation of a ketonic compound and derivative. The process for the asymmetric hydrogenation of a ketonic compound and derivative is characterized in that the asymmetric hydrogenation of said compound is carried out in the presence of an effective amount of a metal complex comprising as ligand an optically active diphosphine corresponding to one of the following formulae: STR1
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- Intramolecular H-Transfer Reactions During the Decomposition of Alkylhydroperoxides in Hydrocarbons as the Solvents
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Eight defined primary and secondary alkylhydroperoxides were decomposed in n-alkanes as the solvent, mostly in the presence of manganese stearate.In all cases the corresponding alcohols and carbonyl compounds were formed as the main products with yields of 60-90percent.Besides, difunctional products were formed by an intramolecular H-transfer in the alkoxy radicals corresponding to the starting hydroperoxides.Products possibly formed by an intramolecular H-transfer in the corresponding alkylperoxy radical could be found only in the case of 4-methyl-2-hydroperoxy pentane.The amount of products formed by intramolecular H-transfer depended on the nature of the C-H bond in δ-position to the original hydroperoxy group and lay between 4percent (primary C-H in the case of 4-hydroperoxy heptane) and 13percent (tertiary C-H in the case of 2-hydroperoxy-5-methyl hexane) with respect to the starting hydroperoxide.The amount of products formed by oxidative attack of the alkoxy and alkylperoxy radicals at the normal paraffins used as the solvents was unexpectedly low (always less than 10percent with respect to the starting hydroperoxide).An increment system is proposed for the calculation of 13C-nmr shifts in alkyl hydroperoxides.
- Jinsheng, Li,Pritzkow, Wilhelm,Voerckel, Volkmar
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- Aromatically substituted azacycloalkyl-alkanediphosphonic acids useful for the treatment of illnesses that can be attributed to calcium metabolism disorders
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Aromatically substituted azacycloalkylalkanediphosphonic acids of the formula STR1 in which R represents an aromatically substituted azacycloaliphatyl radical that is bonded to the group alk by way of a nitrogen atom and that optionally contains an additional nitrogen atom, and alk represents a divalent aliphatic radical, and their salts, can be used for the treatment of illnesses that can be attributed to calcium metabolism disorders. They are manufactured, for example, by reacting a compound of the formula in which X3 represents carboxy, carbamoyl or cyano, with phosphorus acid and phosphorus trichloride and in an intermediate of the formula STR2 obtained by starting from compounds of the formula IV in which X3 represents cyano or carbamoyl and by working up by hydrolysis, or in a salt thereof, replacing the amino group by hydroxy by treatment with nitrous acid.
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- The Autoxidation of Hept-3-yne
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In the reaction mixtures of the oxidation of hept-3-yne with molecular oxygen as products of the attack on the C-C triple bond heptane-3,4-dione, propionic and butyric acids and a very small amount of 2-ethylvaleric acid were found.Hept-2-en-4-one and hept-3-en-5-one were probably present, but could not be identified unambiguously.As in the case of the isomeric octynes the main primary reaction products were the hydroperoxides formed by attack on the C-H bonds in α-position to the CC triple bond.
- Brose, Th.,Pritzkow, W.,Sebald, F.,Voerckel, V.
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p. 951 - 956
(2007/10/02)
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- Regio- and Enantio-selective Reduction of α,γ-Diketones by Fermenting Baker's Yeast
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Reduction of various numbers of 2,4 alkanediones by fermenting baker's yeast has been found to be highly regio- and enantioselective, resulting in the formation of 2-hydroxy-4-alkanones.In some cases, optical purities of the products exceeded over 99percent as determined by HPLC analysis of MTPA esters.The highest yield was obtained when the reaction was carried out at pH 8 with low substrate concentration.As the representative β-hydroxyketones, the absolute configuration of (+)-2-hydroxy-4-octanone (2d) and (+)-3-hydroxy-1-phenyl-1-butanone (2h) was unambiguously determined to be (S) by comparing the specific rotation of diol derivatives with those of authentic specimens.
- Ohta, Hiromichi,Ozaki, Kazuhiko,Tsuchihashi, Gen-ichi
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p. 2499 - 2502
(2007/10/02)
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- Chemical process for preparing 1,3 diketones
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Novel (3',5'-dihydrocarbyl-4'-hydroxybenzyl)-1,3-diketones are prepared by reacting an N,N-dihydrocarbyl-2,6-dihydrocarbyl-4-aminomethylphenol with a 1,3-diketone in the presence of a basic substance. The products are useful as antioxidants.
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- Chemical process for preparing 1,3-diketones
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Novel (3',5'-dihydrocarbyl-4'-hydroxybenzyl)-1,3-diketones are prepared by reacting an N,N-dihydrocarbyl-2,6-dihydrocarbyl-4-aminomethylphenol with a 1,3-diketone and an alkyl halide in the presence of an alkali or an alkaline earth metal hydride. The products are useful as antioxidants.
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- PORPHYRINS. 18. SYNTHESIS OF OCTAPROPYLPORPHYRIN BY THE METHOD OF MONOPYRROLE CYCLOTETRAMERIZATION OF 5-CARBOXY-2-METHOXYMETHYL-3,4-DIPROPYLPYRROLE. INVESTIGATION OF THE THERMOLYSIS OF meso-N-METHYLFORMALDIMINEOCTAPROPYLPORPHYRIN
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The synthesis of octapropylporphyrin on the basis of 5-carboxy-2-methoxymethyl-3,4-dipropylpyrrole was realized.It was demonstrated that in the thermolysis of meso-N-methylformaldimineoctapropylporphyrin, 31,51-cyclo-31-ethylidene- and 31,51-cyclo-31-ethyl-51-(N-methylimine) derivatives are also formed in addition to 31,51-cyclo-31-ethylheptapropylporphyrin.
- Shul'ga, A. M.,Ponomarev, G. V.
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p. 748 - 753
(2007/10/02)
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- An Improved Two-step Route for the Preparation of β-Diketones from Aldehydes and its Application to the Synthesis of β-Damascone
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α-Diazo-β-hydroxyketones, obtained by condensation of aldehydes with 1-diazo-1-lithioacetone, are efficiently transformed into the corresponding β-diketones by exposure to rhodium(II) acetate, The sequence is applied to a new synthesis of β-damascone (10).
- Pellicciari, Roberto,Fringuelli, Renata,Sisani, Ettore,Curini, Massimo
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p. 2566 - 2569
(2007/10/02)
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