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ChemicalBook CAS DataBase List Methyl glycolate
96-35-5

Methyl glycolate synthesis

13synthesis methods
Methyl glycolate was synthesized in a single step by reaction of CA with sodium hydroxide and methanol in an autoclave reactor. The highest MG yield of 81.4% was obtained under suitable conditions of 8:1:1 methanol: sodium hydroxide: CA (molar ratio), after 5 h at 150 °C, in a laboratory autoclave reactor.
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Yield:96-35-5 100%

Reaction Conditions:

with C33H32Cl2N2P2Ru;hydrogen;sodium methylate in para-xylene;toluene at 5 - 100; under 37503.8 Torr; for 4 h;Glovebox;Reagent/catalyst;

Steps:

1; 3; 5; 7; 8 Embodiment 8:

In the same experimental procedure as in the fourth embodiment, the catalyst was changed to III-C-1 (26.2 mg).The corresponding product MG yield was obtained as 100%.
In the same manner as in the fourth experimental procedure, the substrate was converted to methyl benzoate (1.03 g) to obtain a yield of the corresponding product benzyl alcohol (BA) of 100%.
In an argon atmosphere glove box,Weigh 25.7 mg of catalyst III-A-1,20.5 mg sodium methoxide,0.89 g of dimethyl oxalate (substrate ester: sodium methoxide: catalyst = 200 : 10 : 1 (molar ratio)),After 6 mL of toluene and 50 μL of p-xylene (internal standard) in a 100 mL reactor,Assemble the kettle and remove the glove box.Then, the kettle was cooled to 5 °C with ice water.The argon gas in the autoclave was replaced with hydrogen (10 bar) three times and then hydrogenated to 50 bar.The kettle was placed in a heating apparatus and heated to 100 ° C and maintained at this temperature for 4 h.After the reaction is completed, the temperature of the kettle body is quickly lowered to 5 ° C and the remaining hydrogen in the kettle is drained.The reaction solution was filtered through a short column of 1 cm silica gel and analyzed by gas chromatography (GC) (KB-Wax column 60 m × 0.32 mm × 0.33 μm).The yields of methyl glycolate (MG) and ethylene glycol (EG) were 86% and 13%, respectively.

References:

CN109776618,2019,A Location in patent:Paragraph 0038; 0040; 0042; 0044; 0046

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