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2-(5-AMINO-3-METHYL-PYRAZOL-1-YL)-ETHANOL synthesis

2synthesis methods
-

Yield:-

Reaction Conditions:

in pentan-1-ol; for 12 h;Heating / reflux;

Steps:

8.a Preparation of 5-amino-1-(β-hydroxyethyl)-3-methylpyrazole

To a solution of 16.4 g (0.2 mol) of 3-aminocrotononitrile in 100 cm3 of n-pentanol were added 16.7 g (0.22 mol) of β-hydroxyethylhydrazine and the mixture was then heated at reflux for 12 hours. The n-pentanol was subsequently distilled off under reduced pressure. A thick oil was obtained, which crystallizes by addition of 150 cm3 of isopropyl ether. A beige solid was obtained, which was filtered off on a sinter funnel. After drying under vacuum at 40° C., 18 g of the expected product were obtained in the form of a beige solid, the melting point of which was from 66 to 68° C.

References:

US6338741,2002,B1 Location in patent:Page column 22