反应详情

A solution of 2-chlorobenzoxazole (15.4 g) in dry tetrahydrofuran (50 ml) was added dropwise to an ice cooled solution of 2-methylaminoethanol (15.0 g) in dry tetrahydrofuran (100 ml) with stirring and protection from atmospheric moisture. The mixture was stirred at 0° C. for 1 hour, allowed to warm to room temperature and stirred for a further 2 hours. The solvent was removed under reduced pressure, the product was dissolved in ethyl acetate (200 ml) and washed with brine (2×150 ml). The organic layer was dried (MgSO4), filtered and the solvent evaporated. Chromatography of the residue on silica-gel in dichloromethane gave the title compound (mp 62°-3° C.) which was used in Preparation 3 without further purification.

1. stirringThe mixture was stirred at 0° C. for 1 hour
2. stirringstirred for a further 2 hours
3. customThe solvent was removed under reduced pressure
4. dissolutionthe product was dissolved in ethyl acetate (200 ml)
5. washwashed with brine (2×150 ml)
6. dry with materialThe organic layer was dried (MgSO4)
7. filtrationfiltered
8. customthe solvent evaporated