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39488-46-5

2-CYANO-N-PENTYLACETAMIDE synthesis

4synthesis methods
-

Yield:39488-46-5 53.1%

Reaction Conditions:

for 12 h;Reflux;

Steps:

7.1 Example 7

1) In a 250 ml three-necked flask, 5 g of cyanoacetic acid, 40 ml of ethanol, and 0.1 g of thionyl chloride were refluxed for 5 h; after completion of the reaction, the mixture was cooled to room temperature and 20 ml of a 0.5 μg aH(3) 3 solution was added. Then, 20 ml of petroleum ether was added to extract the organics, and the organic layer was washed 3 times with saturated NaCl solution and water, then dried over anhydrous MgS04 and filtered. The crude product obtained by the above operation was separated and purified by column chromatography. The eluate used was petroleum ether:ethyl acetate=4:1 (by volume), and the product was a pale yellow liquid. In a 250 ml three-neck flask was added 2 g of the above product, 26 mmol of pentylamine, refluxed for 12 h. After filtration, the precipitate was recrystallized from ethanol to give the product as a needle-like white solid, 2.09 g of 2-cyanoacetylpentylamine, with a yield of 53.1%.

References:

CN107011318,2017,A Location in patent:Paragraph 0008; 0114; 0115