Claims Analysis
Total Claims: 18
Claim 1
Independent Claim
315 words
A process for the preparation of an optically active N-mercaptoalkanoylamino acid represented by formula (I): ##STR16## wherein R 1 is lower alkyl having from 1 to 4 carbon atoms, Y is (CH 2 ) n , n being 1 or 2, or sulfur, and Q is hydroxy or the residual part of an amino acid represented by formula (II): ##STR17## wherein R 2 is lower alkyl having from 1 to 4 carbon atoms or benzyl, which comprises (1) reacting an optically active β-hydroxyalkanoic acid represented by formula (III): ##STR18## wherein R 1 is the same as defined above, with thionyl chloride or thionyl bromide in the presence of a catalyst by keeping the temperature of the reaction mixture at not more than 25° C. when said thionyl chloride or thionyl bromide is mixed with the compound (III) and then raising the temperature of the reaction mixture up to from about 30° C. to about 100° C. to prepare an optically active β-haloalkanoyl halide represented by formula (IV): ##STR19## wherein X is chlorine or bromine and R 1 is the same as defined above; (2) reacting the β-haloalkanoyl halide with an amino acid represented by formula (V): ##STR20## wherein Y and Q are the same as defined above, to produce an optically active N-β-haloalkanoylamino acid represented by formula (VI): ##STR21## wherein X, R 1 , Y and Q are the same as defined above; and (3) reacting the N-β-haloalkanoylamino acid with an alkali metal salt of hydrogen sulfide or ammonium hydrosulfide, of which the molar ratio to the compound (VI) is from about 2 to about 10, in water or a polar aprotic solvent at a temperature of from about 60° C. to about 90° C., the configuration of the formulas (II), (III), (IV), (V), and (VI) being retained in all the optically active compounds throughout the process to prepare the compound represented by formula (I).
Claim 2
Dependent Claim
315 words
A process for the preparation of an optically active N-mercaptoalkanoylamino acid represented by formula (I): ##STR16## wherein R 1 is lower alkyl having from 1 to 4 carbon atoms, Y is (CH 2 ) n , n being 1 or 2, or sulfur, and Q is hydroxy or the residual part of an amino acid represented by formula (II): ##STR17## wherein R 2 is lower alkyl having from 1 to 4 carbon atoms or benzyl, which comprises (1) reacting an optically active β-hydroxyalkanoic acid represented by formula (III): ##STR18## wherein R 1 is the same as defined above, with thionyl chloride or thionyl bromide in the presence of a catalyst by keeping the temperature of the reaction mixture at not more than 25° C. when said thionyl chloride or thionyl bromide is mixed with the compound (III) and then raising the temperature of the reaction mixture up to from about 30° C. to about 100° C. to prepare an optically active β-haloalkanoyl halide represented by formula (IV): ##STR19## wherein X is chlorine or bromine and R 1 is the same as defined above; (2) reacting the β-haloalkanoyl halide with an amino acid represented by formula (V): ##STR20## wherein Y and Q are the same as defined above, to produce an optically active N-β-haloalkanoylamino acid represented by formula (VI): ##STR21## wherein X, R 1 , Y and Q are the same as defined above; and (3) reacting the N-β-haloalkanoylamino acid with an alkali metal salt of hydrogen sulfide or ammonium hydrosulfide, of which the molar ratio to the compound (VI) is from about 2 to about 10, in water or a polar aprotic solvent at a temperature of from about 60° C. to about 90° C., the configuration of the formulas (II), (III), (IV), (V), and (VI) being retained in all the optically active compounds throughout the process to prepare the compound represented by formula (I).
Claim 3
Dependent Claim
20 words
The process according to claim 1 wherein R 1 is methyl, Y is CH 2 , and Q is hydroxy.
Claim 4
Dependent Claim
18 words
The process according to claim 1 wherein R 1 is methyl, Y is sulfur, and Q is hydroxy.
Claim 5
Dependent Claim
32 words
The process according to claim 1 wherein R 1 is methyl, Y is CH 2 , and Q is the residual part of an amino acid (II) wherein R 2 is benzyl.
Claim 6
Dependent Claim
24 words
The process according to claim 1 wherein the molar ratio of the catalyst to the compound (III) is from about 0.0001 to about 0.1.
Claim 7
Dependent Claim
19 words
The process according to claim 1 wherein the catalyst is an organic amine or an acid addition salt thereof.
Claim 8
Dependent Claim
24 words
The process according to claim 6 wherein the organic amine is methylamine, dimethylamine, trimethylamine, ethylamine, diethylamine, triethylamine, imidazole, piperidine, morpholine, pyridine, N,N-dimethylaniline, or N,N-diethylaniline.
Claim 9
Dependent Claim
14 words
The process according to claim 1 wherein the catalyst is an organic acid amide.
Claim 10
Dependent Claim
20 words
The process according to claim 8 wherein the organic acid amide is formamide, N-methylformamide, N,N-dimethylformamide, acetamide, N,N-dimethylacetamide, N-formylmorpholine, or N-formylpiperidine.
Claim 11
Dependent Claim
27 words
The process according to claim 1 wherein the molar ratio of thionyl chloride or thionyl bromide to the compound (III) is from about 2 to about 3.
Claim 12
Dependent Claim
21 words
The process according to claim 1 wherein the halogenation of the compound (III) is carried out in an inert organic solvent.
Claim 13
Dependent Claim
25 words
The process according to claim 11 wherein the inert organic solvent is diethyl ether, tetrahydrofuran, methylene chloride, ethylene dichloride, chloroform, carbon tetrachloride, benzene, or toluene.
Claim 14
Dependent Claim
17 words
The process according to claim 1 wherein the polar aprotic solvent is dimethyl sulfoxide, N,N-dimethylformamide, or N,N-dimethylacetamide.
Claim 15
Dependent Claim
32 words
The process according to claim 1 wherein the concentration of the alkali metal salt of hydrogen sulfide in the reaction system is from about 5 wt % to about 10 wt %.
Claim 16
Dependent Claim
28 words
The process according to claim 1, wherein the conversion of the halogen in the compound (VI) into the thiol group is carried out in an inert gas atmosphere.
Claim 17
Dependent Claim
42 words
The process according to claim 1 wherein the optically active β-hydroxyalkanoic acid (III) is prepared by subjecting the corresponding alkanoic acid to the action of a microorganism having the ability to convert the alkanoic acid into the optically active β-hydroxyalkanoic acid (III).
Claim 18
Dependent Claim
45 words
The process according to claim 2 wherein the optically active β-hydroxyalkanoic acid (III) is prepared by subjecting isobutyric acid or methacrylic acid to the action of a microorganism having the ability to convert isobutyric acid or methacrylic acid into the optically active β-hydroxyalkanoic acid (III).