Welcome to chemicalbook!
Chinese English Japanese Germany Korea
400-158-6606
Try our best to find the right business for you.
Do not miss inquiry messages Please log in to view all inquiry messages.

Welcome back!

ChemicalBook CAS DataBase List 3-Fluoro-4-methylbenzoic acid
350-28-7

3-Fluoro-4-methylbenzoic acid synthesis

9synthesis methods
-

Yield:350-28-7 84%

Reaction Conditions:

Stage #1:carbon dioxide with o-phenylenebis(diphenylphosphine);copper(II) acetate monohydrate in 1,4-dioxane at 60; for 0.416667 h;Schlenk technique;
Stage #2:2-fluoro-4-bromotoluene with palladium diacetate;triethylamine;4,5-bis(diphenylphosphino)-9,9-dimethylxanthene in 1,4-dioxane;toluene at 100; for 4 h;Schlenk technique;

Steps:

9 Preparation of benzoic acid
General procedure: In a Schlenk (50 mL) reaction flask with a carbon dioxide balloon attached to a branch tube, add Cu (OAc) 2.H2O (0.0125 mmol), 1,2-bis (diphenylphosphine) benzene (0.018 mmol), and 1,4 -Dioxane (2.0mL), PMHS (2.5mmol) was added under stirring, and then the reaction flask was placed in an oil bath at 60 ° C for 25min to react under carbon dioxide atmosphere, followed by toluene (8mL) and bromobenzene (1.0 mmol), Pd (OAc) 2 (0.03 mmol), 4,5-bisdiphenylphosphine-9,9-dimethylxanthene (0.06 mmol), Et3N (2.5 mmol, 2.5 equiva.), The carbon dioxide was then removed and reacted at 100 ° C until the raw bromobenzene disappeared. After cooling to room temperature, sodium hydroxide solution (1M, 10.0mL) was added, stirred for 10min, and filtered. The solid was washed three times with water, and the filtrate was washed with ethyl acetate ( 2 × 10mL) left after extraction, the aqueous layer was adjusted to pH 1-2 with hydrochloric acid solution (1M), extracted with ethyl acetate (3 × 15mL), dried over anhydrous sodium sulfate,The solvent was removed to give benzoic acid. Yield, 65%.

References:

Dalian Institute of Chemical Physics;Li Can;Lu Shengmei;Ku Malasiwami·palidala;Wang Mengmeng CN110724047, 2020, A Location in patent:Paragraph 0085-0086; 0109-0111; 0176

FullText

3-Fluoro-4-methylbenzoic acid Related Search: