反应详情

2-Nitro-5-(2,4-dichlorophenoxy)aniline (1.6 g, 5.4 mmol) is dissolved in a solution of potassium hydroxide (0.33 g, 5.9 mmol) in ~150 ml of ethanol. The mixture is cooled to -5°, and sodium hypochlorite (17 ml of 5.3% solution, 0.9 g, 11.8 mmol) is added dropwise over 20 minutes. The reaction is stirred at RT overnight, then cooled to 10° and ~2 ml of sodium hypochlorite is added. One hour later, the reaction is stripped. The residue is taken up in ether, washed with water, dried, stripped and purified by prep. TLC (10% ethyl acetate/hexane) to yield 5-(2,4-dichlorophenoxy)benzo-2,1,3-oxadiazole N-oxide, m.p. 92°-93°.

1. temperatureThe mixture is cooled to -5°
2. temperaturecooled to 10°
3. customOne hour
4. washwashed with water
5. customdried
6. custompurified by prep