反应详情

A reaction vessel fitted with a calcium sulfate drying tube was charged with 4.9 g (55 mmol) of 2-amino-2-methyl-1-propanol and 50 ml of anhydrous ethyl ether. With this mixture stirred at 0°-5° C., there was added dropwise over a period of 45 minutes a solution of 50 ml anhydrous ethyl ether containing 6.5 g (25 mmol) of 2-(tert-butylamino)-4-trifluoromethyl-5-oxazolecarbonyl chloride. The reaction mixture was stirred at ambient temperature for 11/2 hours, then filtered to remove the HCl salt of 2-amino-2-methyl1-propanol. The ether filtrate was washed successively with one molar oxalic acid and saturated brine, then dried under magnesium sulfate, and concentrated under reduced pressure to yield 8.2 g of a colorless, viscous oil. This oil was mixed with hexane and heated to reflux to yield a white solid material. The material was cooled and filtered to yield 7.7 g of a white crystalline product (m.p.=140°-144° C.) identified in Table I.

1. customA reaction vessel fitted with a calcium sulfate drying tube
2. stirringThe reaction mixture was stirred at ambient temperature for 11/2 hours
3. filtrationfiltered
4. customto remove the HCl salt of 2-amino-2-methyl1-propanol
5. washThe ether filtrate was washed successively with one molar oxalic acid and saturated brine
6. customdried under magnesium sulfate
7. concentrationconcentrated under reduced pressure
8. customto yield 8.2 g of a colorless, viscous oil
9. temperatureheated
10. temperatureto reflux
11. customto yield a white solid material
12. temperatureThe material was cooled
13. filtrationfiltered