Phosphorus oxychloride → 2-Chloro-4,6-dimethyl-5-nitropyrimidine

A mixture of Compound 1 (500 mg) and phosphorus oxychloride (3.89 g) was stirred for 3 hours under reflux. After the reaction was completed, the mixture was concentrated under reduced pressure. To the resulting residue, chloroform and water were added and the mixture was cooled and neutralized with a 2N aqueous sodium hydroxide solution to a pH of 5 to 7. The mixture was then extracted with chloroform and the organic layer was concentrated under reduced pressure to obtain 411 mg of the desired product. When necessary, some of the product was purified by silica gel column chromatography (ethyl acetate:hexane=1:1) to give a purified product.

1. temperatureunder reflux
2. concentrationthe mixture was concentrated under reduced pressure
3. additionTo the resulting residue, chloroform and water were added
4. temperaturethe mixture was cooled
5. extractionThe mixture was then extracted with chloroform
6. concentrationthe organic layer was concentrated under reduced pressure

ORDレコード

ord-ddc622b86f36401fb4eabe652680dd57

出典データセット

uspto-grants-2013_11

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08592435B2