Ethanol → 3-Methoxy-isonicotinic acid

A mixture of 0.89 g of 3-methoxymethyl isonicotinonitrile, 0.72 g of sodium hydroxide, 6 ml of ethanol and 6 ml of water was heated to reflux for three hours. The reaction mixture was cooled to room temperature, and concentrated under reduced pressure. 3 Mhydrochloric acid was added so that pH of the resultant residue became about 3. The reaction mixture was concentrated under reduced pressure. To the resultant solid, 40 ml of ethanol was added. The mixture was heated to reflux for five minutes, and subjected to hot filtration. The solid collected by filtration was subjected to the same operation twice by using 40 ml each of ethanol. Combined filtrates were concentrated to give 1.0 g of 3-methoxy isonicotinic acid.

1. temperaturewas heated
2. temperatureto reflux for three hours
3. concentrationconcentrated under reduced pressure
4. addition3 Mhydrochloric acid was added so that pH of the resultant residue
5. concentrationThe reaction mixture was concentrated under reduced pressure
6. additionTo the resultant solid, 40 ml of ethanol was added
7. temperatureThe mixture was heated
8. temperatureto reflux for five minutes
9. filtrationsubjected to hot filtration
10. filtrationThe solid collected by filtration
11. concentrationCombined filtrates were concentrated

ORDレコード

ord-7e1daf76d2fa4e598c427f9104f44708

出典データセット

uspto-grants-2012_12

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08324387B2