2,3-Lutidine → Pyridine, 2,3-dimethyl-, 1-oxide

温度

0 °C

In methylene chloride (200 ml) was dissolved 2,3-dimethylpyridine (9.50 g) and the resulting solution was. cooled to 0° C. Metachloroperbenzoic acid (21.9 g) was added to the reaction mixture, followed by heating to room temperature. Stirring was conducted for 3 days. An aqueous solution of sodium sulfite was added and the resulting mixture was separated using methylene chloride (200 ml). The organic layer was dried over anhydrous magnesium sulfate, the filtrate was concentrated and the concentrate was purified by chromatography on a silica gel column (5% methanol—methylene chloride). Petroleum ether was added to the residue. Colorless powder so precipitated was collected by filtration, followed by drying, whereby the title compound (5.47 g) was obtained.

1. temperatureby heating to room temperature
2. customthe resulting mixture was separated
3. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
4. concentrationthe filtrate was concentrated
5. customthe concentrate was purified by chromatography on a silica gel column (5% methanol—methylene chloride)
6. additionPetroleum ether was added to the residue
7. customColorless powder so precipitated
8. filtrationwas collected by filtration
9. customby drying

ORDレコード

ord-68e958ca661d45c6ae2ebf8889725afc

出典データセット

uspto-grants-2004_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06747023B1