ethyl 2-methyl-1,3-dioxolane-2-propionate synthesis
- Product Name:ethyl 2-methyl-1,3-dioxolane-2-propionate
- CAS Number:941-43-5
- Molecular formula:C9H16O4
- Molecular Weight:188.22
Yield:941-43-5 100%
Reaction Conditions:
with trimethylsilyl trifluoromethanesulfonate in dichloromethane at -78; for 4.5 h;
Steps:
1.A Example 1: Chemical Synthesis of Fluorinated VPA Analogues A) Preparation of sodium 4,4-difluoro-2-propylpentanoate (7). Preparation of ethyl 3-(2-methyl-1,3-dioxolan-2-yl) propanoate (2)
A pre-cooled mixture (-78°C) of TMSOTf (1.56 g) in CH2Cl2 (7 ml) was treated with 1, 2-bis (triethylsilyloxy) ethane (16. 33 g) and ethyl levulinate (10.09 g) respectively under nitrogen, and the reaction mixture was stirred for 4.5 h. The reaction mixture was treated with pyridine, the organic layer was separated, the aqueous phase was extracted with ethyl acetate, and the combined organic extracts were washed with brine and dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by vacuum distillation to give 12.9 g of compound 2 as a colourless liquid having bp 63°C/0. 3 mmHg.
References:
WO2004/54957,2004,A2 Location in patent:Page 23-24
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