2-CYANO-4-PYRIDINE CARBOXYLIC ACID METHYL ESTER synthesis
- Product Name:2-CYANO-4-PYRIDINE CARBOXYLIC ACID METHYL ESTER
- CAS Number:94413-64-6
- Molecular formula:C8H6N2O2
- Molecular Weight:162.15
Yield:94413-64-6 94%
Reaction Conditions:
with copper(l) iodide;N,N-Dimethylcarbamoyl chloride in acetonitrile at 80; for 5 h;
Steps:
1 Example 1: Preparation of the compound of formula (4) Methyl 2-cyanoisonicotinate
The formula (5) compound methyl isobutyl niacin-N-oxide 1.53g (10mmol), b a carbamic chloride (0.11 ml, 11mmol), zinc cyanide (1.40g, 12mmol), cuprous iodide 0.19g (1mmol) dissolved in 50 ml of acetonitrile, mixtures in 80 °C reaction under 5 hours, TLC detection reaction (hexane/ethyl acetate = 1 the [...] 1), after the reaction, cooling to room temperature, add 20 ml water to stir reaction 5-30 minutes, removed the organic layer, the aqueous layer extracted with ethyl acetate three times, each 50 ml, combined with the organic layer, anhydrous sodium sulfate for drying, distilling solvent under reduced pressure, to obtain crude products, crude product using normal hexane/ethyl acetate = 4 the [...] 1 column chromatography, to obtain strawcoloured solid 1.53g, yield 94%, HPLC purity ( unitary method ): 97.7% ; melting point: 107.5-108.7 °C.
References:
CN104151297,2016,B Location in patent:Paragraph 0037; 0038
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