ChemicalBook CAS DataBase List 3-Pyridinecarboxylic acid, 1,2-dihydro-2-thioxo-, Methyl ester

3-Pyridinecarboxylic acid, 1,2-dihydro-2-thioxo-, Methyl ester synthesis

6synthesis methods

Product Name:3-Pyridinecarboxylic acid, 1,2-dihydro-2-thioxo-, Methyl ester
CAS Number:74470-32-9
Molecular formula:C7H7NO2S
Molecular Weight:169.2

67-56-1 Synthesis

67-56-1
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38521-46-9 Synthesis

38521-46-9
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3-Pyridinecarboxylic acid, 1,2-dihydro-2-thioxo-, Methyl ester

74470-32-9
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Yield:74470-32-9 205 g

Reaction Conditions:

with sodium hydrogen sulfate at 112; for 2.5 h;Temperature;

Steps:

1; 2 Example 1

191 g of 2-mercapto-3-pyridinecarboxylic acid, 32 g of methanol, and 2 g of sodium hydrogen sulfate were put into a reactor, stirred, and heated to 112 ° C, and the reaction was continued for 2.5 hours under a vacuum of -0.06 MPa to remove the generated water, followed by washing with water. Sodium hydrogen sulfate,Dehydration to obtain 205 g of methyl mercaptobenzoate;The above reaction product methyl mercaptopicolinate and 186 g of lauryl alcohol were reacted in a 10% sodium hydroxide solution at 85 ° C for 2-3 hours, washed with water to remove methanol and alkali, and dehydrated to obtain decyl pyridyl picolinate 359 g. The product was mixed with 165 g of dipropylene glycol methyl ether at 60-65 ° C for 30 minutes, and then added with barium hydroxide 104 g, and the temperature was raised to 85 ° C, and a 30% aqueous ammonia solution was added dropwise to a pH of 6 or more, and the reaction was carried out for 3.5 hours. The layers were separated, the oil phase was dehydrated, and filtered to obtain a nitrogen-containing fatty alcohol ester sulfonium salt. The barium content was determined to be 11.32%

References:

CN110229097,2019,A Location in patent:Paragraph 0029-0032