ChemicalBook CAS DataBase List 2-Mercaptothiazoline

2-Mercaptothiazoline synthesis

8synthesis methods

Product Name:2-Mercaptothiazoline
CAS Number:96-53-7
Molecular formula:C3H5NS2
Molecular Weight:119.21

75-15-0
251 suppliers
$40.00/100g

926-39-6
150 suppliers
$14.00/5g

141-43-5 Synthesis

141-43-5
885 suppliers
$9.00/10g

96-53-7
314 suppliers
$6.00/10g

Yield:96-53-7 97 %

Reaction Conditions:

in water at 45 - 55;Industrial scale;

Steps:

1-6

(1) Weigh the raw materials according to the proportion, the molar ratio of 2-aminoethyl sulfate, ethanolamine, carbon disulfide and water is 1:1.02:1.1:22;(2) Dilute ethanolamine at a concentration of 99% with water at a mass ratio of about 1:1 to a 50% aqueous solution of ethanolamine for later use;(3) 900 kilograms of 2-aminoethyl sulfate, 250 kilograms of ethanolamine aqueous solution of 50% concentration and 2050 kilograms of water are added in the 5000L ring-closure reactor, after stirring and dissolving, stop stirring, close all valves;(4) Open the vacuum valve, vacuumize the ring-closing reactor with a vacuum pump, close the vacuum valve to stop vacuuming when the vacuum degree reaches-0.98MPa, and then slowly add 533.6 kilograms of carbon disulfide at one time;(5) Control the reaction temperature in the range of 45 to 55°C, then slowly add 544 kilograms of ethanolamine aqueous solution with a concentration of 50% for reaction, which can be achieved by the steam or cooling water and the drop rate of the jacket of the ring-closing reactor and the internal cooling coil Control the reaction temperature; after the dropwise addition is completed, continue to keep warm for 30 minutes; during the reaction process, the evaporated carbon disulfide is continuously condensed and refluxed into the ring-closure reactor;(6) After the reaction is completed, slowly pass steam and heat up to 83° C. to evaporate and recover excessive carbon disulfide;(7) After the recovery is completed, cool down to below 28°C, open the bottom valve, put the material into the bag filter for filtration, and spray and wash the filter cake according to the ratio of 1 ton of filter cake to 1 ton of water to obtain 736 kg of product The yield of 2-mercaptothiazoline is 97%. The mother liquor obtained by filtering is the wastewater solution of ethanolamine sulfate, and the pH value is 7.6.

References:

CN114989111,2022,A Location in patent:Paragraph 0035-0081