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ChemicalBook CAS DataBase List METHYL 5-METHYLPYRAZINE-2-CARBOXYLATE

METHYL 5-METHYLPYRAZINE-2-CARBOXYLATE synthesis

5synthesis methods
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Yield: 93%

Reaction Conditions:

AMBERLYST for 20 h;Heating / reflux;

Steps:

1 EXAMPLE 1
EXAMPLE 1 The reaction is carried out, under nitrogen, in a 1 L*4 neck flask equipped with a mechanical stirrer, water condenser (with gas inlet), and a thermocouple. The reactor is charged with 5-methylpyrazinecarboxylic acid (100 g), AMBERLYST 15 ion exchange resin (20 g), and methanol (300 g). The mixture is stirred at reflux for about 20 h. After the reaction is complete (analyze with GC or GC/MS), the resin is removed by pressure filtration. The resin is rinsed with methanol. About 75% of the solvent is removed under reduced pressure and the resulting suspension is allowed to stand at room temperature overnight, and then in an ice bath for 3 h. The solid is collected by filtration and washed with ice-cold methanol (2*80 g). Drying under vacuum (25 inches of Hg) yielded 102.4 g (93%) of 5-methyl-2-pyrazonecarboxylic acid, methyl ester that is suitable for use as is.

References:

ISP INVESTMENTS INC. US2005/239803, 2005, A1 Location in patent:Page/Page column 2

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