反应详情

Stir a mixture of triphenylphosphine (3.16 g, 12.06 mmol), bromine (1.91 g, 12.06) and methylene chloride (150 mL) at room temperature for 20 minutes. To the mixture, add a solution of imidazole (0.98 g, 14.48 mmol), 2-Cyclohexyl-N-(2,6-dichloro-4-methoxy-benzyl)-4-hydroxy-butyramide (4.5 g, 12.06 mmol) in methylene chloride (100 mL). Stir the reaction at room temperature for 3.5 hours. Wash the reaction with HCl (1 N), water and brine. After drying the organic layer over sodium sulfate, filter and concentrate under vacuum. Purify the residue by silica gel chromatography with 1:3 ethyl acetate/hexane to afford 2.5 g. of the title compound. MS (m/z): 436 (M+H)+.

1. stirringStir
2. customthe reaction at room temperature for 3.5 hours
3. washWash
4. customthe reaction with HCl (1 N), water and brine
5. dry with materialAfter drying the organic layer over sodium sulfate
6. filtrationfilter
7. concentrationconcentrate under vacuum
8. customPurify the residue by silica gel chromatography with 1:3 ethyl acetate/hexane
9. customto afford 2.5 g