反应详情

To a stirred solution of 27 parts of N-[3,4-dihydro-2-[[(tetrahydro-2H-pyran-2-yl)oxy]methyl]-2H-1-benzopyran-6-yl]-acetamide in 240 parts of methanol were added 100 parts of a hydrochloric acid solution 10% in water. The whole was stirred for 30 minutes at room temperature. The reaction mixture was evaporated till all traces of methanol were removed. After cooling, the product was filtered off from the aqueous phase, washed with water and crystallized from acetonitrile. The product was filtered off and dried, yielding 14.4 parts (74%) of N-[3,4-dihydro-2-(hydroxymethyl)-2H-1-benzopyran-6-yl]acetamide; mp. 156.5° C. (intermediate 12).

1. customThe reaction mixture was evaporated till all traces of methanol
2. customwere removed
3. temperatureAfter cooling
4. filtrationthe product was filtered off from the aqueous phase
5. washwashed with water
6. customcrystallized from acetonitrile
7. filtrationThe product was filtered off
8. customdried