A method for purifying polybutylene terephthalate (PBT) includes: providing or receiving initial PBT, in which oligomers and tetrahydrofuran are present; dissolving the initial PBT in hexafluoroisopropanol (HFIP) to form a solution, in which the oligomers are also dissolved in the HFIP; and contacting the solution with compressed CO.sub.2 at a temperature and a pressure, thereby precipitating the purified PBT, resulting from a large portion of the oligomers are still dissolved in the HFIP, in the operation the temperature is in a range of 20 C. to 35 C., and the pressure is in a range of 900 psi to 1400 psi. A device for purifying PBT is also provided.

A method for purifying polybutylene terephthalate (PBT) includes: providing or receiving initial PBT, in which oligomers and tetrahydrofuran are present; dissolving the initial PBT in hexafluoroisopropanol (HFIP) to form a solution, in which the oligomers are also dissolved in the HFIP; and contacting the solution with compressed CO.sub.2 at a temperature and a pressure, thereby precipitating the purified PBT, resulting from a large portion of the oligomers are still dissolved in the HFIP, in the operation the temperature is in a range of 20 C. to 35 C., and the pressure is in a range of 900 psi to 1400 psi. A device for purifying PBT is also provided.

The present invention relates to novel manganese complexes and their use, inter alia, for homogeneous catalysis in (1) the preparation of imine by dehydrogenative coupling of an alcohol and amine; (2) CC coupling in Michael addition reaction using nitriles as Michael donors; (3) dehydrogenative coupling of alcohols to give esters and hydrogen gas (4) hydrogenation of esters to form alcohols (including hydrogenation of cyclic esters (lactones) or cyclic di-esters (di-lactones), or polyesters); (5) hydrogenation of amides (including cyclic dipeptides, lactams, diamide, polypeptides and polyamides) to alcohols and amines (or diamine); (6) hydrogenation of organic carbonates (including polycarbonates) to alcohols or hydrogenation of carbamates (including polycarbamates) or urea derivatives to alcohols and amines; (7) dehydrogenation of secondary alcohols to ketones; (8) amidation of esters (i.e., synthesis of amides from esters and amines); (9) acylation of alcohols using esters; (10) coupling of alcohols with water and a base to form carboxylic acids; and (11) preparation of amino acids or their salts by coupling of amino alcohols with water and a hydrogenative coupling of alcohols and amines; (13) preparation of imides from diols.

##STR00001## ##STR00002##

The present invention relates to novel manganese complexes and their use, inter alia, for homogeneous catalysis in (1) the preparation of imine by dehydrogenative coupling of an alcohol and amine; (2) CC coupling in Michael addition reaction using nitriles as Michael donors; (3) dehydrogenative coupling of alcohols to give esters and hydrogen gas (4) hydrogenation of esters to form alcohols (including hydrogenation of cyclic esters (lactones) or cyclic di-esters (di-lactones), or polyesters); (5) hydrogenation of amides (including cyclic dipeptides, lactams, diamide, polypeptides and polyamides) to alcohols and amines (or diamine); (6) hydrogenation of organic carbonates (including polycarbonates) to alcohols or hydrogenation of carbamates (including polycarbamates) or urea derivatives to alcohols and amines; (7) dehydrogenation of secondary alcohols to ketones; (8) amidation of esters (i.e., synthesis of amides from esters and amines); (9) acylation of alcohols using esters; (10) coupling of alcohols with water and a base to form carboxylic acids; and (11) preparation of amino acids or their salts by coupling of amino alcohols with water and a hydrogenative coupling of alcohols and amines; (13) preparation of imides from diols.

##STR00001## ##STR00002##

A simple production process is provided of a perfluoroalkyl compound that uses monohydroperfluoroalkane as a starting material, the perfluoroalkyl compound being an important intermediate of organic electronic materials, medicine, agricultural chemicals, functional polymer materials and the like. With monohydroperfluoroalkane is reacted a base and then a carbonyl compound to produce an alcohol having a perfluoroalkyl group. For example, potassium hydroxide is made to interact with trifluoromethane, and a reaction with a carbonyl compound is induced to produce an alcohol having a trifluoromethyl group.

A simple production process is provided of a perfluoroalkyl compound that uses monohydroperfluoroalkane as a starting material, the perfluoroalkyl compound being an important intermediate of organic electronic materials, medicine, agricultural chemicals, functional polymer materials and the like. With monohydroperfluoroalkane is reacted a base and then a carbonyl compound to produce an alcohol having a perfluoroalkyl group. For example, potassium hydroxide is made to interact with trifluoromethane, and a reaction with a carbonyl compound is induced to produce an alcohol having a trifluoromethyl group.

Compositions including 1-chloro-2,2-difluoroethane, and the uses thereof. A composition including 1-chloro-2,2-difluoroethane and at least one additional compound selected from 1,1-difluoroethylene, 1,1,1-trifluoroethane, chlorotrifluoroethylene, 1-chloro-1-fluoroethylene, 1,1-difluoroethane, trans-1-chloro-2-fluoroethylene, 1-chloro-2,2,2-trifluoroethane, 1-chloro-1,2,2-trifluoroethane, cis-1-chloro-2-fluoroethylene, 2,2-dichloro-1,1,1-trifluoroethane, 1,1-dichloro-1-fluoroethane, 1,1-dichloroethylene, 1,2-dichloro-1-fluoroethylene, 1,1-dichloro-2-fluoroethylene, 1,2-dichloro-1,1-difluoroethane, 1,1-dichloro-2,2-difluoroethane, cis-1,2-dichloroethylene, 1,2,2-trichloro-1,1-difluoroethane, 1,1,1-trichloroethane, 1,1-dichloroethane, 1,1,2-trichloro-1-fluoroethane, trichloroethylene, 1,1,2-trichloro-2-fluoroethane, 1,1,2-trichloroethane, 1,1,2,2-tetrachloro-1-fluoroethane, tetrachloroethylene, 1,1,1,2-tetrachloroethane, 1,1,2,2-tetrachloroethane, 1,1,1,2,2-pentachloroethane, tetrachloromethane, 1,2,2-trichloro-1-fluoroethylene, isomers of chloropropene, 1,2-dichloro-1-fluoroethylene, 1-chloro-2-fluoroethane, 1-chloro-1-fluoroethane, 1,1-chloro-2,2,2-trifluoroethane, 1,1,1-trichloro-2,2-difluoroethane, 1-chloroethylene, 1-fluoroethylene, H.sub.2O and HCl; the composition including at least 30% by weight of 1-chloro-2,2-difluoroethane, based on the total weight of the composition.

Compositions including 1-chloro-2,2-difluoroethane, and the uses thereof. A composition including 1-chloro-2,2-difluoroethane and at least one additional compound selected from 1,1-difluoroethylene, 1,1,1-trifluoroethane, chlorotrifluoroethylene, 1-chloro-1-fluoroethylene, 1,1-difluoroethane, trans-1-chloro-2-fluoroethylene, 1-chloro-2,2,2-trifluoroethane, 1-chloro-1,2,2-trifluoroethane, cis-1-chloro-2-fluoroethylene, 2,2-dichloro-1,1,1-trifluoroethane, 1,1-dichloro-1-fluoroethane, 1,1-dichloroethylene, 1,2-dichloro-1-fluoroethylene, 1,1-dichloro-2-fluoroethylene, 1,2-dichloro-1,1-difluoroethane, 1,1-dichloro-2,2-difluoroethane, cis-1,2-dichloroethylene, 1,2,2-trichloro-1,1-difluoroethane, 1,1,1-trichloroethane, 1,1-dichloroethane, 1,1,2-trichloro-1-fluoroethane, trichloroethylene, 1,1,2-trichloro-2-fluoroethane, 1,1,2-trichloroethane, 1,1,2,2-tetrachloro-1-fluoroethane, tetrachloroethylene, 1,1,1,2-tetrachloroethane, 1,1,2,2-tetrachloroethane, 1,1,1,2,2-pentachloroethane, tetrachloromethane, 1,2,2-trichloro-1-fluoroethylene, isomers of chloropropene, 1,2-dichloro-1-fluoroethylene, 1-chloro-2-fluoroethane, 1-chloro-1-fluoroethane, 1,1-chloro-2,2,2-trifluoroethane, 1,1,1-trichloro-2,2-difluoroethane, 1-chloroethylene, 1-fluoroethylene, H.sub.2O and HCl; the composition including at least 30% by weight of 1-chloro-2,2-difluoroethane, based on the total weight of the composition.

Problem to be Solved

It is intended to provide an industrially preferable fluoroalkylating agent and use thereof.

Solution

The present invention provides a fluoroalkylating agent represented by the general formula (1) wherein R.sup.1 is a C1 to C8 fluoroalkyl group; R.sup.2 and R.sup.3 are each independently a C1 to C12 alkyl group or the like; Y.sup.1 to Y.sup.4 are each independently a hydrogen atom, a halogen atom, or the like; and X.sup. is a monovalent anion.

##STR00001##

A compound of the general formula (3): R.sup.4SR.sup.1 having an introduced C1 to C8 fluoroalkyl group is easily obtained by reacting a compound of the general formula (2): R.sup.4SZ wherein R.sup.4 is a hydrocarbon group or the like; and Z is a leaving group, with the compound of the general formula (1).

Problem to be Solved

It is intended to provide an industrially preferable fluoroalkylating agent and use thereof.

Solution

The present invention provides a fluoroalkylating agent represented by the general formula (1) wherein R.sup.1 is a C1 to C8 fluoroalkyl group; R.sup.2 and R.sup.3 are each independently a C1 to C12 alkyl group or the like; Y.sup.1 to Y.sup.4 are each independently a hydrogen atom, a halogen atom, or the like; and X.sup. is a monovalent anion.

##STR00001##

A compound of the general formula (3): R.sup.4SR.sup.1 having an introduced C1 to C8 fluoroalkyl group is easily obtained by reacting a compound of the general formula (2): R.sup.4SZ wherein R.sup.4 is a hydrocarbon group or the like; and Z is a leaving group, with the compound of the general formula (1).