ChemicalBook CAS DataBase List 4-(3-ACRYLOYLOXY-N-PROP-1-YLOXY)BENZOIC ACID

4-(3-ACRYLOYLOXY-N-PROP-1-YLOXY)BENZOIC ACID synthesis

8synthesis methods

Product Name:4-(3-ACRYLOYLOXY-N-PROP-1-YLOXY)BENZOIC ACID
CAS Number:245349-46-6
Molecular formula:C13H14O5
Molecular Weight:250.25

The preparation of 4-(3-acryloyloxy-n-prop-1-yloxy)benzoic acid is as follows:8.1g Allyl 4- (3- (acryloyloxy) propoxy) benzoic acid,4.1 g of N-methylaniline,Add 0.28 g of palladium acetate and 0.66 g of triphenylphosphine to 50 mL of acetonitrile, andStir at room temperature overnight. The reaction solution is diluted with ethyl acetate,The extract was washed with 5% hydrochloric acid and saturated brine, dried over anhydrous sodium sulfate, the solid was filtered off, and the solvent was evaporated. The residue is purified by column chromatography (silica gel, developing solvent: dichloromethane) to yield 4.2 g of 4- (3- (Acryloyloxy) propoxy) benzoic acid(Yield: 80.0%, purity (HPLC): 93.0%) was obtained.

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4-(3-ACRYLOYLOXY-N-PROP-1-YLOXY)BENZOIC ACID

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Yield:245349-46-6 94 g

Reaction Conditions:

with methanesulfonic acid;2,6-di-tert-butyl-4-methyl-phenol in hexane at 70 - 80;

Steps:

1 Synthesis of intermediate 2

Insert stirrer, a reflux condenser, distillation, fractional distillation tube, the intermediate 1 In a reaction vessel equipped with a thermometer 98g (500mmol), methyl acrylate, 1290g, hexane 75g, 70% methanesulfonic acid 14g, butylhydroxytoluene 1.2g, It was reacted under stirring at 70 ~ 80 . The reaction is extracted with methanol produced by the reaction from the top of the distillation column to the fractional distillation tube, it was done until there is no production of methanol. The reaction solution was subjected to washing until the pH of water in 200ml of water was transferred to a 3 after cooling to room temperature, the separating funnel. The organic phase was concentrated at 65 ~ 75 under atmospheric pressure was added to 100g of toluene to obtain a slurry liquid. After the slurry liquid is separated by filtration, toluene was then washed with hexane and dried under reduced pressure to give 94g of Intermediate 2.

References:

KR2015/13217,2015,A Location in patent:Paragraph 0107-0109

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