反应详情

A mixture of (3-dimethoxymethyl-4-nitro-phenyl)-phenyl-methanone (0.0659 mol) and 5N HCl (40 mL) in CH3Cl (80 mL) was stirred at room temperature overnight. Then the mixture was refluxed for 4 h. After cooling, the organic layer was separated. The organic layer was alkalized by adding dropwise NH4OH. The organic layer was washed with water, dried (MgSO4) and evaporated. The residue (14.6 g) was crystallized from diisopropyl ether/EtOAc (50 mL:20 mL). The precipitate was filtered off, washed with diisopropyl ether/EtOAc, diisopropyl ether and dried in vacuo at 50° C. to yield the title compound as a residue.

1. temperatureThen the mixture was refluxed for 4 h
2. temperatureAfter cooling
3. customthe organic layer was separated
4. additionby adding dropwise NH4OH
5. washThe organic layer was washed with water
6. dry with materialdried (MgSO4)
7. customevaporated
8. customThe residue (14.6 g) was crystallized from diisopropyl ether/EtOAc (50 mL:20 mL)
9. filtrationThe precipitate was filtered off
10. washwashed with diisopropyl ether/EtOAc, diisopropyl ether
11. customdried in vacuo at 50° C.