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ChemicalBook CAS DataBase List 1-METHYL-3-TRIFLUOROMETHYL-2-PYRAZOLIN-5-ONE
1481-02-3

1-METHYL-3-TRIFLUOROMETHYL-2-PYRAZOLIN-5-ONE synthesis

2synthesis methods
Ethyl 4,4,4-trifluoroacetoacetate

372-31-6

Methylhydrazine

60-34-4

1-METHYL-3-TRIFLUOROMETHYL-2-PYRAZOLIN-5-ONE

1481-02-3

0.1 mL of methylhydrazine and 10 mL of anhydrous ethanol were added to a 250 mL three-necked flask, stirred and heated to 50°C. Subsequently, 0.1 mol of ethyl trifluoroacetoacetate was slowly added dropwise. After the dropwise addition was completed, the reaction mixture was heated to reflux for 5 hours. Upon completion of the reaction, the mixture was cooled to promote crystallization. The resulting yellow solid was collected by vacuum filtration and dried. The yield of the final product was 85.8%.

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Yield: 85.8%

Reaction Conditions:

in ethanol at 50; for 5 h;

Steps:

1.1 (1) Preparation of 1-methyl-3-trifluoromethyl-5-pyrazolone intermediate:
0.1 ml of methyl hydrazine and 250 mL three-necked flask, add 10 mL of anhydrous ethanol, stirring heated to 50 C , dropwise 0. 1moL ethyl trifluoroacetoacetate, heating reflux 5 h, cooling crystallization , Vacuum filtration, drying, in a yellow solid; Yield: 85.8%.

References:

Guizhou University;XUE, WEI;GONG, HUA YU;WANG, ZHONG BO;ZHANG, JIAN;LIU, MIN;ZHU, XUE SONG;XIA, LI JUAN;ZHAO, HONG JU;CHEN, YU CN103951663, 2016, B Location in patent:Paragraph 0091; 0092; 0093

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