METHYL 5-AMINO-4-CYANO-3-(2-METHOXY-2-OXOETHYL)THIOPHENE-2-CARBOXYLATE synthesis
- Product Name:METHYL 5-AMINO-4-CYANO-3-(2-METHOXY-2-OXOETHYL)THIOPHENE-2-CARBOXYLATE
- CAS Number:674773-12-7
- Molecular formula:C10H10N2O4S
- Molecular Weight:254.26
Yield:674773-12-7 77%
Reaction Conditions:
with morpholine;sulfur in methanol at 40; for 2 h;Heating / reflux;
Steps:
1A EXAMPLE 1A; methyl 5-amino-4-cyano-3-(2-methoxy-2-oxoethyl)-2-thiophene-carboxylate
EXAMPLE 1A methyl 5-amino-4-cyano-3-(2-methoxy-2-oxoethyl)-2-thiophene-carboxylate Introduce into a reactor 400 kg of dimethyl 3-oxoglutarate, 158 kg of malononitrile and 560 litres of methanol and then, whilst maintaining the temperature of the reaction mixture below 40° C., 199.6 kg of morpholine. Then introduce 73.6 kg of sulphur and subsequently bring the mixture to reflux. After reacting for 2 hours, stop refluxing and add water until precipitation occurs.Filter off the precipitate obtained, wash it and dry it. methyl 5-amino-4-cyano-3-(2-methoxy-2-oxoethyl)-2-thiophenecarboxylate is thereby obtained in a yield of 77% and with a chemical purity of 98%.
References:
US2004/63972,2004,A1 Location in patent:Page 4
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