反应详情

温度

90 °C

tert-butyl{2-[4-(pent-4-en-1-yloxy)phenyl]ethyl}carbamate (Preparation 56, 1.2 g, 3.9 mmol), (3R)-3-[2-(benzyloxy)-5-bromophenyl]-N,N-diisopropyl-3-phenylpropan-1-amine (Prepared according to WO9411337, 1.9 g, 3.9 mmol), palladium acetate (90 mg, 0.4 mmol), tri(o-tolyl)phosphine (200 mg, 0.8 mmol), and diisopropylethylamine (1.0 ml, 5.9 mmol) were mixed in acetonitrile (12 ml), degassed with argon and the heated to 90° C. for 5 hours. The reaction was cooled to room temperature, filtered through Arbocel and solvent removed in vacuo. The residue was taken up in water and ethyl acetate, the organics were separated, dried (magnesium sulphate) and the solvent removed in vacuo, the residue was purified by column chromatography on silica gel eluting with dichloromethane:methanol:880 ammonia (981210.2 to 95151.5 by volume) to furnish the title compound as a pale yellow foam, 2.5 g.

1. customdegassed with argon
2. temperatureThe reaction was cooled to room temperature
3. filtrationfiltered through Arbocel and solvent
4. customremoved in vacuo
5. customethyl acetate, the organics were separated
6. dry with materialdried (magnesium sulphate)
7. customthe solvent removed in vacuo
8. customthe residue was purified by column chromatography on silica gel eluting with dichloromethane