Hydrogen Peroxide → 2-Bromo-6-methylpyridine 1-oxide

温度

90 °C

Hydrogen peroxide (30%, 1.76 mL, 17.4 mmol) was added to a solution of 2-bromo-6-methyl-pyridine (1.0 g, 5.80 mmol) in acetic acid (20 mL), and heated for 24 h at 90° C. The reaction mixture was cooled to ambient temperature, and partitioned between dichloromethane and water. The aqueous phase was separated and extracted with dichloromethane. The combined organic phases were washed thoroughly with water and dried over anhydrous sodium sulfate. Concentration in vacuo afforded 2-bromo-6-methyl-pyridine 1-oxide (820 mg, 75%) as a brown liquid which was used in the next step without further purification.

1. temperatureThe reaction mixture was cooled to ambient temperature
2. custompartitioned between dichloromethane and water
3. customThe aqueous phase was separated
4. extractionextracted with dichloromethane
5. washThe combined organic phases were washed thoroughly with water
6. dry with materialdried over anhydrous sodium sulfate
7. concentrationConcentration in vacuo

ORDレコード

ord-e7ec2c1329ad4d029fdc28cbdb7d8051

出典データセット

uspto-grants-2013_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08524705B2