US2014350286A1PendingUtilityA1

Method for Making Two-Phase Solution of which Phase State Changes as a Result of Temperature Conversion React, and Apparatus for Implementing This

Assignee: JAPAN SCIENCE & TECH AGENCYPriority: Oct 8, 2003Filed: Aug 13, 2014Published: Nov 27, 2014
Est. expiryOct 8, 2023(expired)· nominal 20-yr term from priority
Inventors:Kazuhiro Chiba
C07B 61/00C07C 231/02C07C 67/10C07C 231/12B01J 2219/00599Y10T436/255B01J 2219/00495B01J 2219/00364Y10T436/25375B01J 2219/00585B01J 2219/00308B01J 2219/00686B01J 2219/0072B01J 2219/00481
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Claims

Abstract

A method for making a number (N) of samples react under the same reaction conditions, wherein the samples have a solution where the phase state of a reaction solvent changes in a reversible manner between a two-phase solution state and a uniform solution state when the temperature fluctuates over or under a certain constant temperature, and the processes are carried out sequentially in the following steps: (A) the constant container heating step of heating a number of reaction containers simultaneously and maintaining the reaction containers at a predetermined temperature; (B) the sample heating step of putting a sample in each heated reaction container and of maintaining a two-phase solution at a predetermined temperature; (C) the reaction step of stirring the sample that has been heated to the predetermined temperature so as to gain a uniform solution, which is maintained for a predetermined period of time; (D) the cooling step of cooling the uniform solution without cooling the reaction container after the predetermined period of time has passed so as to gain a two-phase solution within the reaction container. According to the present invention, a method for making a two phase solution of which the phase state changes through temperature conversion react through a number of processes, wherein a chemical process can be carried out on a number of samples under the same conditions in one process apparatus, as well as an apparatus for implementing this can be provided.

Claims

exact text as granted — not AI-modified
1 . (canceled) 
     
     
         2 . A method, comprising:
 heating a material solution comprising a reactant and a two-phase reaction solvent comprising a first phase comprising a nonpolar solvent and a second phase comprising a polar solvent to a reaction temperature in a reaction container;   stirring the material solution, such that the first phase and the second phase of the two-phase reaction solvent dissolve each other to form a one-phase solution;   maintaining the one-phase solution, with stirring, at the reaction temperature for a predetermined period of time, to obtain a one-phase product solution comprising a reaction product; and   cooling the one-phase product solution within the reaction container inside the reaction container to a predetermined temperature below the reaction temperature without cooling the reaction container, to obtain a two-phase product solution comprising a solvent phase comprising the polar solvent and a product phase comprising the reaction product and the nonpolar solvent.   
     
     
         3 . The method of  claim 2 , wherein the cooling comprises adding a solid of which the temperature is lower than that of the reaction into the uniform solution within the reaction container. 
     
     
         4 . The method of  claim 2 , wherein the cooling comprises mixing a compound having a lower boiling point directly into the uniform solution within the reaction container. 
     
     
         5 . The method of  claim 2 , further comprising, after the cooling:
 extracting the product phase from the two-phase product solution.   
     
     
         6 . The method of  claim 5 , wherein the solvent phase remains in the reaction container after extracting the product phase and is employed as the second phase of the two-phase reaction solvent in a subsequent reaction. 
     
     
         7 . The method of  claim 2 , wherein the first phase of the two-phase reaction solvent comprises a cycloalkane compound, and wherein the second phase of the two-phase reaction solvent comprises at least one selected from a nitroalkane, a nitrile, an alcohol, an alkyl halide, a carbonate, an imidazolidinone, a carbodiimide, an ester, a carboxylic acid, an aldehyde, a ketone, an ether, a urea, an amide, and a sulfoxide. 
     
     
         8 . The method of  claim 2 , wherein the first phase of the two-phase reaction solvent is an alkane, a cycloalkane, an alkene, an alkyne, or an aromatic compound. 
     
     
         9 . The method of  claim 2 , wherein the first phase of the two-phase reaction solvent is a cycloalkane compound. 
     
     
         10 . The method of  claim 9 , wherein the cycloalkane compound is cyclohexane. 
     
     
         11 . The method of  claim 9 , wherein the cycloalkane compound is methyl cyclohexane. 
     
     
         12 . The method of  claim 9 , wherein the cycloalkane compound is decalin. 
     
     
         13 . The method of  claim 2 , wherein the second phase of the two-phase reaction solvent is a nitroalkane, a nitrile, an alcohol, an alkyl halide, a carbonate, an imidazolidinone, a carbodiimide, an ester, a carboxylic acid, an aldehyde, a ketone, an ether, a urea, an amide compound, or a sulfoxide. 
     
     
         14 . The method of  claim 13 , wherein the second phase of the two-phase reaction solvent is an amide compound. 
     
     
         15 . The method of  claim 14 , wherein the amide compound is dimethyl formamide. 
     
     
         16 . The method of  claim 13 , wherein the second phase of the two-phase reaction solvent is an imidazolidinone compound. 
     
     
         17 . The method of  claim 16 , wherein the imidazolidinone compound is dimethyl imidazolidinone. 
     
     
         18 . The method of  claim 9 , wherein the second phase of the two-phase reaction solvent is an amide compound. 
     
     
         19 . The method of  claim 9 , wherein the second phase of the two-phase reaction solvent is an imidazolidinone compound.

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