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US 4,845,261 AGranted
Process for bis(substituted phenyl) phosphorohalidates
AssigneeMerck & Co., Inc.
InventorLelia M. Fuentes
Life of this patent
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Abstract
This invention relates to a novel process for preparing bis(substituted phenyl) phosphorohalidates.
Claims11
A process for preparing a phosphorohalidate having the formula:
- ##STR8## wherein R is phenyl or phenyl substituted with 1 to 3 substituents selected from the group consisting of:
- (i) halogen;
- (ii) C.sub.1 -C.sub.6 alkyl;
- (iii) C.sub.1 -C.sub.6 alkoxy;
- (iv) C.sub.1 -C.sub.4 fluorinated alkyl;
- or
- (v) NO.sub.2 ;
- and
- X is chlorine or bromine,
- comprising reacting a phosphorus oxyhalide of the formula POX.sub.3, wherein X is defined as above, with an approximately one-fold to two-fold quantity of a phenol of the formula R--OH, wherein R is defined as above, in the presence of a dialkylaminopyridine or a hydrohalide salt thereof at a temperature of from about 100.degree. up to about the boiling point of the reaction mixture.
7 more elements
A process for preparing bis(2,4-dichlorophenyl)phosphorochloridate having the formula ##STR10## comprising (a) reacting phosphorus oxychloride with an approximately 1.2-fold to 2.0-fold molar quantity of 2,4-dichlorophenol in the presence of 4-dimethylaminopyridine or 4-dimethylaminopyridine hydrochloride at a temperature of about 120.degree.;
- (b) adding hexane at a temperature below the boiling point of hexane;
- (c) removing insoluble material from a resultant solution of the bis(2,4-dichlorophenyl)phosphorochloridate in hexane;
- (d) cooling the solution to a temperature of from about 0.degree. to about -40.degree.;
- and
- (e) collecting the bis(2,4-dichlorophenyl)phosphorochloridate by filtration.
2 more elements
A process comprising
- (a) reacting a phosphorus oxyhalide of the formula POX.sub.3 with an approximately one-fold to two-fold molar quantity of a phenol of the formula R--OH in the presence of a dialkylaminopyridine or a hydrohalide salt thereof at a temperature of from about 100.degree. up to about the boiling point of the reaction mixture;
- (b) adding hexane at a temperature below the boiling point of hexane;
- (c) removing insoluble material from a resultant solution of the phosphorohalidate in the hexane;
- (d) cooling the solution to a temperature of from about 0.degree. to about -40.degree.;
- and
- (e) collecting the phosphorohalidate that crystallizes;
- wherein:
- X is chlorine or bromine;
- and R is phenyl or phenyl substituted with 1 to 3 substituents selected from the group consisting of:
- (i) halogen, (ii) C.sub.1 -C.sub.6 alkyl, (iii) C.sub.1 -C.sub.6 alkoxy, (iv) C.sub.1 -C.sub.4 fluorinated alkyl, and (v) NO.sub.2.
7 more elements
Dependencies are inferred from the claim text.