Sodium hydride → 4-(3-Methoxypropoxy)-2,3-dimethyl-1-oxo-1lambda~5~-pyridine

温度

60 °C

2.0 g (22 mmol) of 3-methoxypropanol was dissolved in 50 ml of dimethyl sulfoxide to obtain a solution. 2.7 g (66 mmol) of sodium hydride was added to this solution at a room temperature. The obtained mixture was stirred at 60° C. for one hour and cooled to a room temperature by allowing to stand, followed by the addition of 3.0 g (19 mmol) of 4-chloro-2,3-dimethylpyridine N-oxide. The obtained mixture was stirred at 40° C. for one hour. After the completion of the reaction, the reaction mixture was distilled to remove the dimethyl sulfoxide. The obtained residue was purified by silica gel column chromatography to obtain 760 mg of 4-(3-methoxypropoxy)-2,3-dimethyl-pyridine N-oxide.

1. customto obtain a solution
2. temperaturecooled to a room temperature
3. stirringThe obtained mixture was stirred at 40° C. for one hour
4. customAfter the completion of the reaction
5. distillationthe reaction mixture was distilled
6. customto remove the dimethyl sulfoxide
7. customThe obtained residue was purified by silica gel column chromatography

ORDレコード

ord-587aa44822454a5f84f794e15d2c9f6d

出典データセット

uspto-grants-1999_12

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05998445