1-Methyl-5-oxo-3-pyrrolidinecarboxylic acid methyl ester synthesis
- Product Name:1-Methyl-5-oxo-3-pyrrolidinecarboxylic acid methyl ester
- CAS Number:59857-86-2
- Molecular formula:C7H11NO3
- Molecular Weight:157.17
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Yield: 106.0 g
Reaction Conditions:
with toluene-4-sulfonic acid in dichloromethane at 50; for 16 h;Reflux;
Steps:
1 Example 1
Preparation of methyl N-methyl-2-pyrrolidone-4-carboxylate
239.9 g of N-methyl-2-pyrrolidone-4-carboxylic acid are initially introduced into 410 g of dichloromethane.
Then, at 50° C., 108.4 g of methanol and 9.6 g of p-toluenesulfonic acid are added and the mixture is stirred at reflux for 16 hours.
When the reaction is complete, the reaction mixture is washed with water and sodium hydrogen carbonate solution, and the aqueous phases are extracted by shaking with chloroform and dried over magnesium sulfate.
Filtration is then carried out, and the solvent is removed on a rotary evaporator and subjected to fractional distillation in vacuo.
The product passes over at a temperature of 121-130° C. at 4 to 7 mbar.
The resulting product has a saponification number of 360.0 mg KOH/g (theory: 356.9 mg KOH/g) and a water content of <0.1% by weight.
This gives 106.0 g of methyl N-methyl-2-pyrrolidone-4-carboxylate.
References:
CLARIANT FINANCE (BVI) LIMITED;Wacker, Andreas;Hess, Joachim;Kupfer, Rainer;Roesch, Alexander US2013/217579, 2013, A1 Location in patent:Paragraph 0078
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![Ethanamine, N-[(3,5-dichlorophenyl)methylene]-2,2-diethoxy-](/CAS/20210305/GIF/1000210-73-0.gif)
1000210-73-0
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59857-86-2
43 suppliers
$45.39/250mg