- METHOD FOR PURIFYING 4-HALO CYCLOHEXANE-1-CARBOXYLIC ACID, AND METHODS FOR PRODUCING PRODUCTS CONTAINING 4- HALO CYCLOHEXANE-1-CARBOXYLIC ACID
-
To provide a method for purifying a 4-halo cyclohexane-1-carboxylic acid which can be highly purified without performing column purification, and a method for producing a product containing the 4-halo cyclohexane-1-carboxylic acid.SOLUTION: There is provided a method for purifying a 4-halo cyclohexane-1-carboxylic acid comprising a crystallization step of subjecting a mixture including a 4-halo cyclohexane-1-carboxylic acid and a 3-halo cyclohexane-1-carboxylic acid to a crystallization operation in a mixed solvent of water and a water-soluble organic solvent or a hydrocarbon solvent to increase a content of the 4-halo cyclohexane-1-carboxylic acid.SELECTED DRAWING: None
- -
-
Paragraph 0037-0038
(2020/03/31)
-
- PROCESS FOR PRODUCING OPTICALLY ACTIVE CARBOXYLIC ACID
-
It has been demanded to provide a process for industrially producing an intermediate for a compound that exhibits an inhibitory effect on activated blood coagulation factor X and is useful as a preventive and/or therapeutic agent for thrombotic diseases. The present invention provides a process for producing the (R-α-phenylethylamine salt of (S)-3-cyclohexene-1-carboxylic acid, comprising reacting 3-cyclohexene-1-carboxylic acid and (R)-α-phenylethylamine using a mixed solvent of water and acetone or a mixed solvent of water and ethyl acetate as a solvent.
- -
-
Page/Page column 13
(2011/10/12)
-
- Erbium triflate in ionic liquids: A recyclable system of improving selectivity in Diels-Alder reactions
-
The efficiency of Er(OTf)3 in promoting the Diels-Alder reactions between different dienes and dienophiles in ionic liquids has been investigated. Compared with the analogous cycloadditions performed in conventional solvents shorter reaction times are required to obtain good/excellent yields. In most cases an enhancement of regio- and endo:exo selectivity was observed. The role of the ionic liquid, as a function of the cationic part, i.e. the imidazolium based or the pyridinium based, is discussed well. The ILs containing the catalyst can be readily separated from the reaction products and recovered in very high purity for direct reuse, up to six cycles.
- Bortolini, Olga,De Nino, Antonio,Garofalo, Angelo,Maiuolo, Loredana,Procopio, Antonio,Russo, Beatrice
-
experimental part
p. 124 - 129
(2011/02/16)
-
- Tandem Diels-Alder/cross-coupling reactions of generated in situ organoindium reagents in a one-pot process
-
[Chemical equation presented] Tandem Diels-Alder/ cross-coupling reactions with organoindium reagents generated in situ from 1-bromo-2,3-butadiene and indium were developed in a one-pot process. [4 + 2] Cycloaddition reactions using organoindium reagents and subsequent Pd-catalyzed cross-coupling reactions provided the rapid synthesis of six-membered carbocycles starting from 1-bromo-2,3-butadiene.
- Mo, Juntae,Kim, Sung Hong,Lee, Phil Ho
-
supporting information; experimental part
p. 424 - 427
(2010/04/24)
-
- A practical new chiral controller for asymmetric Diels-Alder and alkylation reactions
-
(formula presented) The enantiomerically pure hydroxy sulfones (+)- and (-)-2 have been prepared from 1,2-epoxycyclohexane by a simple and practical procedure. The acrylate esters of these alcohols undergo BCl3-catalyzed Diels-Alder reactions with a variety of dienes at -78 to -55°C in CH2Cl2 or C7H8 with high dienophile face selectivity (Table 1). The chiral esters so formed are readily cleaved with recovery of the controllers (+)- or (-)-2. Esters of (+)- and (-)-2 can be converted to Z-polassium enolates and alkylated with high face selectivity.
- Sarakinos, Georgios,Corey
-
p. 1741 - 1744
(2008/02/11)
-
- A new class of analogues of the bifunctional radiosensitizer α-(1-aziridinylmethyl)-2-nitro-1H-imidazole-1-ethanol (RSU 1069): The cycloalkylaziridines
-
A series of compounds related to α-(1-aziridinylmethyl)-2-nitro-1H-imidazole-1-ethanol (RSU 1069, 1) were synthesized and evaluated as selective hypoxic cell cytotoxic agents and as radiosensitizers. The aziridine moiety was replaced with a number of other potential alkylating groups including cycloalkylaziridines and azetidines. The data indicated that modification of the aziridine of 1 resulted in a substantial decrease in the ability of the compounds to selectively kill hypoxic cells. However, these modifications did not affect the compounds' in vitro radiosensitizing activity since many of the derivatives were as potent as 1. All of the compounds that were evaluated in vivo were less toxic than 1, and several members of this series had significant activity. The best compound was trans-α-[[(4-bromotetrahydro-2H-pyran-3-yl)amino]methyl]-2-nitro-1H- imidazole-1-ethanol (18), which, due to its activity and log P value, is a candidate for additional in vivo studies.
- Suto,Stier,Werbel,Arundel-Suto,Leopold,Elliott,Sebolt-Leopold
-
p. 2484 - 2488
(2007/10/02)
-
- Pulsed Infrared Laser Inducement of Multiple Reaction Channels in Ethyl 3-Cyclohexene-1-carboxylate
-
The pulsed CO2 laser-induced reaction of ethyl 3-cyclohexenecarboxylate, a large organic ester with two reaction channels differing by ca. 13 kcal mol-1 in threshold energies, was studied over the 0.02-0.20-torr pressure range.The absorbed laser energy and the reaction probabilities were measured as functions of laser energy, laser intensity, and added bath gas.The reaction product ratio was very dependent on the incident laser energy but almost independent of the laser pulse duration (intensity) at constant fluence.The dependence of the product ratio on the absorbed energy was satisfactorily explained for low fractional reaction by a postpulse model using RRKM rate constants and a broad distribution function (simulated as a Boltzmann distribution) with mean energy equal to the absorbed laser energy.In addition to implying that the internal energy is randomly distributed prior to reaction, the model implies that all, or nearly all, of the molecules absorb the laser energy.Addition of bath gas significantly lowered the reaction probability but had only a minor influence on the product partitioning ratio; these results were also interpreted satisfactorily by the model calculations.The laser-driven secondary reaction of the ethyl acrilate product, even for single-pulse experiments, is important.
- Setser, D. W.,Nguyen, Hanh H.,Danen, Wayne C.
-
p. 408 - 417
(2007/10/02)
-