Acetyl chloride → 4-Chloro-2-methyl-1-oxo-1lambda~5~-pyridine

15.4 g (0.1 mol) of 2-methyl-4-nitropyridine 1-oxide was added to 78.5 g (1 mol) of acetyl chloride at -10° C. The obtained mixture was stirred under cooling with ice for 0.5 hour. After the completion of the reaction, 300 ml of ice-water was added to the reaction mixture. The obtained mixture was neutralized with sodium carbonate and extracted with chloroform. The extract was dried over magnesium sulfate and filtered. The filtrate was concentrated under a reduced pressure and purified by silica gel column chromatography (ethyl acetate/n-hexane/methanol) to obtain 4.7 g of the title compound.

1. temperatureunder cooling with ice for 0.5 hour
2. additionwas added to the reaction mixture
3. extractionextracted with chloroform
4. dry with materialThe extract was dried over magnesium sulfate
5. filtrationfiltered
6. concentrationThe filtrate was concentrated under a reduced pressure
7. custompurified by silica gel column chromatography (ethyl acetate/n-hexane/methanol)

ORDレコード

ord-743aec568dbb4f9fb0d7ff56d8c684aa

出典データセット

uspto-grants-1998_11

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05840910