C07C53/16

Method of producing high-purity monochloroacetic acid
10538474 · 2020-01-21 · ·

A method has been disclosed of obtaining high purity, colourless monochloroacetic acid encompassing the chlorination of acetic acid with chlorine in the presence of a catalyst, followed by the recovery of the catalyst through vacuum distillation and purification of the obtained liquid raw product by its hydrodehalogenation by hydrogen in the presence of a palladium catalyst and then vacuum distillation.

Method of producing high-purity monochloroacetic acid
10538474 · 2020-01-21 · ·

A method has been disclosed of obtaining high purity, colourless monochloroacetic acid encompassing the chlorination of acetic acid with chlorine in the presence of a catalyst, followed by the recovery of the catalyst through vacuum distillation and purification of the obtained liquid raw product by its hydrodehalogenation by hydrogen in the presence of a palladium catalyst and then vacuum distillation.

Cyclobutyl (S)-2-[[[(R)-2-(6-aminopurin-9-yl)-1-methyl-ethoxy]methyl-phenoxy-phosphoryl]amino]-propanoates, and production process and application thereof

The present invention relates to chemotherapeutic agents for the treatment of viral and cancerous diseases. Said compounds are prodrugs of the inhibitors of human immunodeficiency virus (HIV) and hepatitis B virus (HBV) of DNA polymerase and are intended for the treatment of human immunodeficiency virus, hepatitis B and co-infections HIV/HCV, HIV/HBV, HIV/HCV/HBV, and HCV/HBV.

Method of industrially producing monochloroacetic acid
10494325 · 2019-12-03 · ·

A method of producing monochloroacetic acid (MCAA) has been disclosed encompassing (a) a stage of the direct chlorination of acetic acid with chlorine and (b) a stage of recovery of the catalyst in the form of acid chlorides from the reaction mixture before (c) a hydrodehalogenation stage characterized by the fact that the chlorination process (a) is conducted at the boiling temperature of the mixture under a pressure of 0-1.0 barg, in an excess of acetic acid with respect to the dosed chlorine gas, while the heat from the reaction is taken off mainly through the evaporation of volatile components of the mixture, followed by their condensation in the reflux condenser above the reactor and the return to the chlorination reaction, after which the reaction mixture containing monochloroacetic acid, acetic acid, dichloroacetic acid and optionally acid chlorides which are present in the mixture and, optionally, anhydrides of these acids, is feed to the vacuum distillation process (b), which is conducted continuously in the distillation column in a vacuum of 0 to 500 mbar from which volatile components of the mixture, mainly acid chlorides, as well as some acetic acid and some monochloroacetic acid are taken off as distillate and returned to the chlorination process as a result of which the catalyst of the chlorination is almost completely recovered.

Method of industrially producing monochloroacetic acid
10494325 · 2019-12-03 · ·

A method of producing monochloroacetic acid (MCAA) has been disclosed encompassing (a) a stage of the direct chlorination of acetic acid with chlorine and (b) a stage of recovery of the catalyst in the form of acid chlorides from the reaction mixture before (c) a hydrodehalogenation stage characterized by the fact that the chlorination process (a) is conducted at the boiling temperature of the mixture under a pressure of 0-1.0 barg, in an excess of acetic acid with respect to the dosed chlorine gas, while the heat from the reaction is taken off mainly through the evaporation of volatile components of the mixture, followed by their condensation in the reflux condenser above the reactor and the return to the chlorination reaction, after which the reaction mixture containing monochloroacetic acid, acetic acid, dichloroacetic acid and optionally acid chlorides which are present in the mixture and, optionally, anhydrides of these acids, is feed to the vacuum distillation process (b), which is conducted continuously in the distillation column in a vacuum of 0 to 500 mbar from which volatile components of the mixture, mainly acid chlorides, as well as some acetic acid and some monochloroacetic acid are taken off as distillate and returned to the chlorination process as a result of which the catalyst of the chlorination is almost completely recovered.

Deprotection method
10442834 · 2019-10-15 · ·

The present invention provides a method of efficiently deprotecting a protected organic compound by catalytic hydrogenation. Specifically, the present invention provides a method of deprotecting an organic compound having at least one functional group selected from the group consisting of a carboxy group, an amino group and a hydroxy group, which is protected by a protecting group represented by the formula (I):
R.sup.1C(R.sup.2)(R.sup.3)-L.sup.1-(I)
[wherein R.sup.1 is an aryl group optionally having substituent(s), R.sup.2 and R.sup.3 are each independently, a hydrogen atom or an aryl group optionally having substituent(s), and L.sup.1 is a single bond, OCO or OCH.sub.2], comprising hydrogenation in the presence of a metal catalyst and halogenated acetic acid.

Deprotection method
10442834 · 2019-10-15 · ·

The present invention provides a method of efficiently deprotecting a protected organic compound by catalytic hydrogenation. Specifically, the present invention provides a method of deprotecting an organic compound having at least one functional group selected from the group consisting of a carboxy group, an amino group and a hydroxy group, which is protected by a protecting group represented by the formula (I):
R.sup.1C(R.sup.2)(R.sup.3)-L.sup.1-(I)
[wherein R.sup.1 is an aryl group optionally having substituent(s), R.sup.2 and R.sup.3 are each independently, a hydrogen atom or an aryl group optionally having substituent(s), and L.sup.1 is a single bond, OCO or OCH.sub.2], comprising hydrogenation in the presence of a metal catalyst and halogenated acetic acid.

COMPOSITIONS COMPRISING DICHLOROACETIC ACID, PROCESSES FOR PREPARING SAME AND USES THEREOF

A composition comprising dichloroacetic acid and glyoxylic acid, wherein, the content of glyoxylic acid is below 1000 pm, and the preparation method and application of the composition. A process for preparing the composition, comprising: mixing a dichloroacetic acid material having greater than 1000 ppm glyoxylic acid with a glyoxylic acid capture reagent, and a process for preparing oligonucleotides, comprising using the composition. It is found that glyoxylic acid is an impurity in commercially available DCA products, which may cause the oligonucleotides synthesis failure. Ion chromatography can be used to detect glyoxylic acid in dichloroacetic acid and accurately determine its concentration.

COMPOSITIONS COMPRISING DICHLOROACETIC ACID, PROCESSES FOR PREPARING SAME AND USES THEREOF

A composition comprising dichloroacetic acid and glyoxylic acid, wherein, the content of glyoxylic acid is below 1000 pm, and the preparation method and application of the composition. A process for preparing the composition, comprising: mixing a dichloroacetic acid material having greater than 1000 ppm glyoxylic acid with a glyoxylic acid capture reagent, and a process for preparing oligonucleotides, comprising using the composition. It is found that glyoxylic acid is an impurity in commercially available DCA products, which may cause the oligonucleotides synthesis failure. Ion chromatography can be used to detect glyoxylic acid in dichloroacetic acid and accurately determine its concentration.

Method Of Producing High-Purity Monochloroacetic Acid
20190062252 · 2019-02-28 · ·

A method has been disclosed of obtaining high purity, colourless monochloroacetic acid encompassing the chlorination of acetic acid with chlorine in the presence of a catalyst, followed by the recovery of the catalyst through vacuum distillation and purification of the obtained liquid raw product by its hydrodehalogenation by hydrogen in the presence of a palladium catalyst and then vacuum distillation.