反应详情

(3-amino-4-chloro-2-methylphenoxy)acetonitrile (4.76 g) was dissolved in pyridine (45 mL) under an atmosphere of nitrogen and cooled in an ice bath. Methanesulfonyl chloride (2.06 mL) was added dropwise, and then the mixture was allowed to stir overnight at room temperature. The reaction mixture was evaporated to dryness under reduced pressure to afford a residue which was flash chromatographed on silica and eluted with, first ethyl acetate:hexane (1:2), then with ethyl acetate: hexane (1:1) to afford 5.36 g as an 80:20 mixture of mono and bis mesylated product, respectively. This mixture was used in the next step without any further purification.

1. temperaturecooled in an ice bath
2. customThe reaction mixture was evaporated to dryness under reduced pressure
3. customto afford a residue which
4. customchromatographed on silica
5. washeluted with, first ethyl acetate:hexane (1:2)
6. customwith ethyl acetate: hexane (1:1) to afford 5.36 g
7. additionas an 80:20 mixture of mono and bis
8. customThis mixture was used in the next step without any further purification