ChemicalBook CAS DataBase List 2-Mercapto-4-methyl-5-thiazoleacetic acid

2-Mercapto-4-methyl-5-thiazoleacetic acid synthesis

5synthesis methods

Product Name:2-Mercapto-4-methyl-5-thiazoleacetic acid
CAS Number:34272-64-5
Molecular formula:C6H7NO2S2
Molecular Weight:189.26

513-74-6

123-76-2

2-Mercapto-4-methyl-5-thiazoleacetic acid

34272-64-5

To the reactor were added 100 kg of acetylpropionic acid and 1000 L of carbon tetrachloride. Under stirring conditions, 176 kg of sodium bromide was added, followed by a slow dropwise addition of 260 kg of hydrogen peroxide solution. The reaction mixture was heated to 60 °C and maintained at this temperature for 2.5 hours. Upon completion of the reaction, water was added for washing to separate the organic and aqueous phases. The aqueous phase was treated as waste water. To the organic phase, 75 kg of ammonium dithiocarbamate, 1000 kg of water and 22 kg of sodium carbonate were added directly to the organic phase to carry out the cyclization reaction. After completion of the reaction, the aqueous phase was acidified with acid at pH=1.5 to precipitate the product. Finally, 132 kg of 2-mercapto-4-methyl-5-thiazoleacetic acid was obtained with 99.92% purity and 80.99% yield.

513-74-6 Synthesis

513-74-6
169 suppliers
$5.00/1g

123-76-2 Synthesis

123-76-2
491 suppliers
$5.00/25g

34272-64-5
182 suppliers
$13.00/1g

Yield: 80.99%

Reaction Conditions:

Stage #1:levulinic acid with dihydrogen peroxide;sodium bromide in tetrachloromethane at 60; for 2.5 h;Large scale;
Stage #2:ammonium dithiocarbamate with sodium carbonate in tetrachloromethane;waterLarge scale;Reagent/catalyst;Temperature;Solvent;

Steps:

2 Example 2
Add 100kg of levulinic acid and 1000L of carbon tetrachloride to the reactor.After adding 176 kg of sodium bromide and stirring, slowly add 260 kg of hydrogen peroxide solution.Heat to 60°C for 2.5 hours, add water to wash, and separate organic phase.The aqueous phase treats the wastewater. To the organic phase, 75 kg of ammonium dithiocarbamate, 1000 kg of water, and 22 kg of sodium carbonate were directly added for the cyclization reaction.The aqueous phase is acidified with pH=1.5, obtaining2-mercapto-4-methyl-5-thiazoleacetic acid 132 kg, purity 99.92%,Yield 80.99%.

References:

Shandong Jincheng Pharmaceutical And Chemical Co., Ltd.;Sun Tingting;Du Hanyue;Ma Yongxiang;Zhao Qi;Li Shanshan CN107602503, 2018, A Location in patent:Paragraph 0024; 0025; 0026; 0027; 0028; 0029-0034