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REFERENCE EXAMPLE 3 Synthesis of 2-methyl-4-trifluoromethylthiazole-5-carbonyl chloride 0.50 g of <strong>[117724-63-7]2-methyl-4-trifluoromethylthiazole-5-carboxylic acid</strong> was added to 5 ml of thionyl chloride and reaction was carried out for 2 hours under reflux. After the reaction, the reaction mixture was concentrated to obtain 0.54 g of 2-methyl-4-trifluoromethylthiazole-5-carbonyl chloride.
10.7 g
With thionyl chloride; In 1,2-dichloro-ethane; for 0.5h;Reflux;
to the reaction of <strong>[117724-63-7]2-methyl-4-trifluoromethyl-thiazole-5-carboxylic acid</strong> (0.048mol) and 1, 2-dichloroethane (80 ml), stirring 0.5hr rear, adds by drops two chlorine Asia sulphone (0.102mol), reaction under reflux conditions after the drop finishes 3-4hr, removing solvent to obtain orange red liquid title object 10.7 g.
18.5 g
With thionyl chloride; In dichloromethane; at 35℃;
<strong>[117724-63-7]2-methyl-4-trifluoromethylthiazole-5-carboxylic acid</strong> (100 mmol),Thionyl chloride (150 mmol) and 1,2-dichloroethane (100 mL)React at 3-5 hrs at 35C to the system reflow temperature,Removal of the solvent afforded the title compound (18.5 g).
With bis(trichloromethyl) carbonate; In N,N-dimethyl-formamide; toluene; at 50℃; for 1.25h;
52.8 g (0.25 mol) of <strong>[117724-63-7]2-methyl-4-trifluoromethyl-5-thiazolecarboxylic acid</strong> was added to the reaction vessel. 33.4g (0.112mol) of triphosgene, dissolved in 100mL of toluene, and added 1g (0.014mol) of N,N-dimethylformamide at 50 C, and the addition time is 15min. After the addition is completed, it is added dropwise. The acid chloride reaction was carried out for 1 h at a temperature.
REFERENCE EXAMPLE 2 Synthesis of 2-methyl-4-trifluoromethylthiazole-5-carboxylic acid 1.3 g of ethyl 2-methyl-4-trifluoromethylthiazole-5-carboxylate and 0.4 g of potassium hydroxide were dissolved in a mixture of 5 ml each of water and ethanol and reaction was effected at room temperature overnight. After the reaction, the reaction mixture was concentrated and acidified with dilute hydrochloric acid and extracted with ethyl acetate. The extract was concentrated to obtain 0.89 g of 2-methyl-4-trifluoromethylthiazole-5-carboxylic acid.
21.5 g
With sodium hydroxide; In ethyl acetate; at 40℃; for 1h;
115 g of ethyl 2-methyl-4- (trifluoromethyl) thiazole-5-carboxylate (0.102 mol)Of ethyl acetate solution,50 g of a 40% sodium hydroxide solution was added dropwise to the reaction vessel at room temperature,Dropping speed was controlled so that the internal temperature of the system was lower than 40 C,After the dropwise addition of the sodium hydroxide solution,Insulation reaction 60min.After heat preservation,Taking the organic phase,To this was slowly added 10% hydrochloric acid,Adjusted to the system PH ? 2,At this point a large number of estimates of precipitation,The product was filtered,The filter cake was washed twice with 10% hydrochloric acid and dried in a vacuum oven.Methyl-4- (trifluoromethyl) thiazole-5-carboxylic acid as a light yellow solid, 21.5 g of 2-methyl-4- (trifluoromethyl) 98.8%, and the reaction yield was 98.70%.
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