反应详情

To a stirred and cooled (10° C.) solution of 13.7 parts of intermediate 57, namely [4-amino-3-[[(tetrahydro-2H-pyran-2-yl)oxy]methyl]phenyl] phenylmethanone, in 147 parts of pyridine were added dropwise 7.14 parts of ethyl chloroformate. After stirring for 1 hour at 10° C., the reaction mixture was poured into 700 parts of water. The product was extracted with dichloromethane and the extract was washed with water (3×), dried, filtered and evaporated. The residue was co-evaporated with ethanol (3×) and was then crystallized from ethanol. The product was filtered off, washed with ethanol and 2,2'-oxybispropane and dried in vacuo at 60° C., yielding 14.05 parts (83.5%) of ethyl [4-benzoyl-2-[[(tetrahydro-2H-pyran-2-yl)oxy]methyl]phenyl]carbamate; mp. 115.9° C. (interm. 58).

1. stirringAfter stirring for 1 hour at 10° C.
2. extractionThe product was extracted with dichloromethane
3. washthe extract was washed with water (3×)
4. customdried
5. filtrationfiltered
6. customevaporated
7. customwas then crystallized from ethanol
8. filtrationThe product was filtered off
9. washwashed with ethanol and 2,2'-oxybispropane
10. customdried in vacuo at 60° C.