m-Chloroperbenzoic acid → 2-Bromo-5-methylpyridine 1-oxide

温度

50 °C

A mixture of 2-bromo-5-methylpyridine (2.0 g, 11.6 mmol) and 3-chloroperbenzoic acid (3.0 g, 14.8 mmol) in chloroform (7 mL) was stirred at 50° C. for 3 hours, cooled down to room temperature and filtered. The filtrate was concentrated under reduced pressure to give a residue that was purified by flash chromatography (Si—PPC, MeOH:EtOAc, gradient 0:100 to 10:90) to give 2-Bromo-5-methylpyridine 1-oxide as a white solid (2.0 g, 91%). 1H NMR (400 MHz, CHCl3-d): δ 8.24 (s, 1 H); 7.52 (d, J=8.3 Hz, 1 H); 6.93 (d, J=8.33 Hz, 1 H); 2.29 (s, 3 H).

1. temperaturecooled down to room temperature
2. filtrationfiltered
3. concentrationThe filtrate was concentrated under reduced pressure
4. customto give a residue that
5. customwas purified by flash chromatography (Si—PPC, MeOH:EtOAc, gradient 0:100 to 10:90)

ORDレコード

ord-e68fabc155d44350bcdbc314b690daf9

出典データセット

uspto-grants-2012_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08173650B2