m-Chloroperbenzoic acid → 3-Chlorobenzoic Acid

m-Chloroperbenzoic acid, 77% (1.53 g; 6.8 mmol) was added to a solution of A2.5 (1.23 g; 6.5 mmol) in 60 ml of chloroform at rt. After stirring 1 hr at rt, additional m-chloroperbenzoic acid, 77% (75 mg; 0.3 mmol) was added and the reaction mixture was stirred 2 hrs. Following one more addition of m-chloroperbenzoic acid, 77% (40 mg; 0.18 mmol) and one hr of stirring, the reaction mixture was concentrated to a salmon colored solid. Trituration with ethyl ether and filtration afforded 1.5 g (>100%; contaminated with 3-chlorobenzoic acid) of A2.6 as a salmon colored solid.

1. stirringthe reaction mixture was stirred 2 hrs
2. stirringof stirring
3. concentrationthe reaction mixture was concentrated to a salmon
4. filtrationTrituration with ethyl ether and filtration

ORD record

ord-4226d64cbab74d1586ed262286c0df44

Source dataset

uspto-grants-2010_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07683171B2