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ChemicalBook CAS DataBase List METHYL HYDROGEN PHTHALATE
4376-18-5

METHYL HYDROGEN PHTHALATE synthesis

12synthesis methods
-

Yield:4376-18-5 99%

Reaction Conditions:

with 5 wt percent zeolite NaY-Bf at 180; for 5 h;Autoclave;Green chemistry;

Steps:

Methylation of carboxylic acids with dimethylcarbonate. General procedure

General procedure: Into a stainless steel pressure microreactor of capacity 17 mL was charged 5 wt % of zeolite NaY-Bf, 100 mmol of carboxylic acid, and 300-400 mmol of dimethyl carbonate, the reactor was hermetically closed, and the reaction mixture was heated at 180-200°C for 5 h. On completion of the reaction the reactor was cooled to room temperature, opened, the reaction mixture was filtered through a bed of Al2O3. Unreacted dimethyl carbonate was distilled off, the residue was distilled at atmospheric pressure or in a vacuum, or it was crystallized from ethanol.

References:

Khusnutdinov;Shchadneva;Mayakova, Yu. Yu.;Konovalova, Yu. S.;Khazipova;Kutepov [Russian Journal of Organic Chemistry,2017,vol. 53,# 2,p. 163 - 168][Zh. Org. Khim.,2017,vol. 53,# 2,p. 177 - 181,5]

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