反应详情

温度

50 °C

To a solution of 251 mg of 1-(S)-(1-(R)-(3,5-bis(trifluoromethyl)-phenyl)ethoxy)-2-(S)-(4-fluorophenyl)-3-(R)-(methylamino)cyclopentane from Example 15 in 6 mL of acetonitrile was added 0.108 mL of t-butyl bromoacetate and 0.36 mL of DIPEA. The reaction was heated at 50° C. for 5 hours and then concentrated in vacuo. The residue was diluted with water and extracted twice with ethyl acetate. The organic layers were washed with brine, dried with sodium sulfate, combined and evaporated. The residue was purified by FC (0-2.5% methanol in methylene chloride) to afford 294 mg of title compound. Mass spec (ESI): 564 (M+1).

1. concentrationconcentrated in vacuo
2. additionThe residue was diluted with water
3. extractionextracted twice with ethyl acetate
4. washThe organic layers were washed with brine
5. dry with materialdried with sodium sulfate
6. customevaporated
7. customThe residue was purified by FC (0-2.5% methanol in methylene chloride)