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ChemicalBook CAS DataBase List 2-Methyl-1,3-dioxolane-2-propanoic Acid
4388-57-2

2-Methyl-1,3-dioxolane-2-propanoic Acid synthesis

12synthesis methods
-

Yield:4388-57-2 86%

Reaction Conditions:

with 1.3 wt% Na-β zeolite (Na/Al ratio: 0.5; Si/Al ratio: 25) in cyclohexane at 120; for 1 h;Dean-Stark;

Steps:

2.4. Preparation of ketals from ethyl levulinate with polyols

General procedure: In a typical reaction, a mixture of ethyl levulinate (1 g, 6.94 mmol),polyol (1-2 mole ratio w.r.t carbonyl compounds), 10 wt% of -zeolitecatalyst w.r.t. EL (100 mg), and cyclohexane (5 mL) were taken in a 20mL reaction tube. The reaction was carried out in METLER TOLEDOEasy Max 102 glass reactor with the help of Dean-Stark setup at 120 C(for ethylene glycol) or 140 C (for glycerol) at 1000 rpm for 1 h (forethylene glycol) or 4 h (for glycerol). After the reaction, the solid catalystwas separated from product mixture by centrifugation and the supernatantliquid was rotatory evaporated to remove the cyclohexanesolvent. The obtained liquid products were characterized by 13C NMR.Conversion of reactants and yield of products were analysed by Varian450 gas chromatograph (GC) with a flame ionization detector (FID). Theconditions for gas chromatography were as follows: ZB-5MS column, 30m × 0.25 mm × 0.25 m; carrier gas: nitrogen; injection temperature,250 C; detector temperature, 350 C; oven temperature, 80 C to 220 Cat a programmed heating rate of 20 C/min and 5 min hold at 220 C.

References:

Gundekari, Sreedhar;Mani, Mariappan;Mitra, Joyee;Srinivasan, Kannan [Molecular catalysis,2022,vol. 524,art. no. 112269]

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