反应详情

温度

0 °C

To a solution of 29.6 g of 5-amino-2-methylbenzoxazole in 100 ml pyridine cooled to 0° C. was added 41.3 g hexanesulfonyl chloride. After 1 hour stirring at 0° C., a reddish precipitate formed. The reaction mixture was stirred at room temperature for 2 days and then poured into 1.4 l of water and stirred for 2 hours. A heavy oil deposited and the supernatant was decanted. The oil was dissolved in 1.0 l dichloromethane, which was extracted with 4×200 ml of 1N hydrochloric acid, then dried over magnesium sulfate. The solvent was removed, leaving a reddish brown liquid of 5-hexylsulfonamido-2-methylbenzoxazole (Intermediate A).

1. customa reddish precipitate formed
2. stirringThe reaction mixture was stirred at room temperature for 2 days
3. stirringstirred for 2 hours
4. customthe supernatant was decanted
5. dissolutionThe oil was dissolved in 1.0 l dichloromethane
6. extractionwhich was extracted with 4×200 ml of 1N hydrochloric acid
7. dry with materialdried over magnesium sulfate
8. customThe solvent was removed