反应详情

Treat a mixture of 2,6-dichloro-4-methoxy-benzylamine hydrochloride (4.0 g, 16.6 mmol) and toluene (100 mL) with trimethylaluminum (2 M in toluene, 16.6 mL, 33.2 mmol) at room temperature for 10 minutes. To the mixture, add a solution of 3-cyclohexyl-dihydro-furan-2-one (2.51 g, 14.94 mmol) in toluene (50 mL). Stir the reaction at reflux for 6 hours. Cool the reaction and quench with HCl (1 N, 50 mL). Partition the mixture with ethyl acetate and HCl (1 N). Separate the organic layer and wash with water and brine. After drying the organic layer over sodium sulfate and filtration, concentrate the filtrate to afford 4.5 g (81%) of the title compound as white solid. MS (m/z): 374 (M+H)+.

1. additionTreat
2. customthe reaction
3. temperatureat reflux for 6 hours
4. temperatureCool
5. customthe reaction
6. customquench with HCl (1 N, 50 mL)
7. customPartition the mixture with ethyl acetate and HCl (1 N)
8. customSeparate the organic layer
9. washwash with water and brine
10. customAfter drying the organic layer
11. filtrationover sodium sulfate and filtration
12. concentrationconcentrate the filtrate