反应详情

2-(3-{3-[[2-chloro-3-(trifluoromethyl)benzyl)(2,2-diphenylethyl)-amino]-propoxy}-phenyl acetic acid (50 mg, 0.086 mmole) and morpholine (8.7 mg, 0.10 mmole) were dissolved in CH3CN (2 ml). BOP reagent (44 mg, 0.10 mmole) was added followed by Et3N (20 mg, 0.20 mmole). The resultant mixture was stirred at room temperature for 2 h. The mixture was concentrated under reduced pressure. The residue was partitioned between EtOAc and aqueous Na2CO3 (5%) solution. The organic layer was separated, dried over MgSO4 and concentrated. In cases where the product required further purification, a preparative Gilson HPLC was used (YMC CombiPrep ODS-A, 50×20 mm, 20 ml/min, 30–90% CH3CN over 15 minutes). The HCl salt was made by adding HCl (in ether) to an ether solution of the product and then evaporation of the solvent to give a yellow solid (32 mg, 54%). MS(ES) m/e 651.2 [M+H]+.

1. concentrationThe mixture was concentrated under reduced pressure
2. customThe residue was partitioned between EtOAc and aqueous Na2CO3 (5%) solution
3. customThe organic layer was separated
4. dry with materialdried over MgSO4
5. concentrationconcentrated
6. customIn cases where the product required further purification
7. custom(YMC CombiPrep ODS-A, 50×20 mm, 20 ml/min, 30–90% CH3CN over 15 minutes)
8. additionby adding HCl (in ether) to an ether solution of the product
9. customevaporation of the solvent