反应详情

To a stirred and cooled (0° C.) mixture of 4.5 parts of 2-amino-2-methyl-1-propanol and 130 parts of dichloromethane were added portionwise 4.93 parts of 4-(phenylmethoxy)benzoyl chloride. Upon complete addition, stirring was continued for 48 hours at room temperature. The precipitate was filtered off and the filtrate was evaporated. The residue was stirred in 2,2'-oxybispropane. The precipitated product was filtered off and stirred in 9.6 parts of thionyl chloride during 1 hour. After evaporation, the residue was taken up in a sodium hydroxide solution 10%, crushed ice and methylbenzene. The separated organic layer was washed with water, dried, filtered and evaporated, yielding 5 parts (90%) of 4,5-dihydro-4,4-dimethyl-2-[4-(phenylmethoxy)phenyl]oxazole as a residue (int. 1).

1. temperaturecooled
2. additionUpon complete addition
3. stirringstirring
4. filtrationThe precipitate was filtered off
5. customthe filtrate was evaporated
6. stirringThe residue was stirred in 2,2'-oxybispropane
7. filtrationThe precipitated product was filtered off
8. stirringstirred in 9.6 parts of thionyl chloride during 1 hour
9. customAfter evaporation
10. customcrushed ice and methylbenzene
11. washThe separated organic layer was washed with water
12. customdried
13. filtrationfiltered
14. customevaporated