反应详情

1-[4-Amino-3,5-dichlorophenyl]-2-bromoethanone (0.95 g), N-[3-[2-(3-phenoxypropoxy)ethoxy]propyl]benzenemethanamine (1.15 g) and DEA (0.48 g) were stirred together in THF (35 ml) at room temperature under nitrogen for 7 h. The mixture was filtered and the filtrate evaporated in vacuo. The residue was dissolved in methanol (35 ml) and treated portionwise with sodium borohydride (0.34 g), at 0° C. under nitrogen, stirred at room temperature for 18 h, diluted with water (150 ml) and the solvent evaporated in vacuo. The residue was extracted with ethyl acetate (2×150 ml), dried and evaporated in vacuo to give an oil. Purification by FCC eluting with System H (95:5:1) gave the title compound (1.30 g) as an oil. T.l.c. (System H 90:10:1) Rf 0.39

1. filtrationThe mixture was filtered
2. customthe filtrate evaporated in vacuo
3. dissolutionThe residue was dissolved in methanol (35 ml)
4. additiontreated portionwise with sodium borohydride (0.34 g), at 0° C. under nitrogen
5. additiondiluted with water (150 ml)
6. customthe solvent evaporated in vacuo
7. extractionThe residue was extracted with ethyl acetate (2×150 ml)
8. customdried
9. customevaporated in vacuo
10. customto give an oil
11. customPurification by FCC
12. washeluting with System H (95:5:1)