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ChemicalBook CAS DataBase List (4-CHLORO-5-METHYL-3-TRIFLUOROMETHYL-PYRAZOL-1-YL)-ACETIC ACID

(4-CHLORO-5-METHYL-3-TRIFLUOROMETHYL-PYRAZOL-1-YL)-ACETIC ACID synthesis

2synthesis methods
-

Yield:378758-70-4 89%

Reaction Conditions:

with lithium hydroxide monohydrate;water in tetrahydrofuran at 60; for 5 h;

Steps:

b

To a solution of ethyl 2-(4-chloro-5-methyl-3-(trifluoromethyl)-1H-pyrazol-1-yl)acetate (7.5 g, 27.7 mmol) in THF (100 mL) and water (50 mL) was added LiOH.H2O (2.33 g, 55.4 mmol). The mixture was stirred at 60° C. for 5 hours. After cooling to room temperature, the mixture was acidified with 1 N HCl (80 mL) and extracted with 1:2 IPA/CHCl3 (2×150 mL). The combined organic layers were washed with brine, dried (Na2SO4), filtered, and concentrated in vacuo to give the desired compound (6 g, 24.7 mmol, 89%). 1H NMR (400 MHz, DMSO-d6) δ 4.98 (s, 2H), 2.21 (s, 3H); MS: (ES) m/z calculated for C7H6ClF3N2O2 [M+H]+ 243.0, found 243.0

References:

US2014/57937,2014,A1 Location in patent:Paragraph 0093; 0095

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