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2-methyl-2-(4-methylphenoxy)propanoic acid synthesis

6synthesis methods
-

Yield:23438-11-1 8.393 g

Reaction Conditions:

with sodium hydroxide in chloroform at 50; for 1 h;

Steps:

13 2-methyl-2- (4-methylphenoxy) propanoic acid

added to the feed in 1000mL three bottles methyl phenol 11. 431g (0. 106mol), 503mL (6. 85mol) of acetone and sodium hydroxide 62. 640g (l. 566mol), connect the device, insert the thermometer, stirring 10min, the reaction solution was white turbid, 20 ° C was added dropwise under chloroform 40. 5mL (0. 498mol), the reaction solution was gradually warmed until boiling, the reaction solution turns yellow, ice-water bath until the temperature drops to 50 71/92 ° C or less, lh drop was completed, then gradually cooled reflux for 3h, TLC showed that the product no longer point increase, to stop the reaction.Red semi-solid was concentrated under reduced pressure was added 200mL of water, adjust pH3, a white precipitate was extracted with chloroform (20mLX3), separated, adjusted to pH 8 with saturated sodium bicarbonate, water extraction (90mLX3), separated, and water is added 10 pH was adjusted to 3% HC1 to precipitate a lot of white precipitate was extracted with chloroform (20mLX3), dried over anhydrous Na2S04, filtered to remove the drying agent and concentrated to give a yellow oil, was added 5mL of cyclohexane, the freezer overnight, the precipitated needle-like crystals, pumping filter, cyclohexane wash (5mLX3), and dried to give a white solid 8 · 393g

References:

CN102532123,2016,B Location in patent:Paragraph 0215-0216; 0219; 0220

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