反应详情

p-Toluenesulfonic acid monohydrate (6.00 mg, 0.0338 mmol) was added to methyl 4-{(1S)-1-[({2,5-dichloro-4-[(3-chlorophenyl)(tetrahydro-2H-pyran-2-yloxy)methyl]-3-thienyl}carbonyl)amino]ethyl}benzoate from Example 8, Step 4 (197 mg, 0.338 mmol) in MeOH (2 mL). After 1.5 h, the reaction mixture was quenched with 5% aq. NaHCO3 and extracted with EtOAc. The combined organics were washed with 5% aq. NaHCO3, water and brine, dried (Na2SO4) and concentrated. The crude product was purified by Combi Flash chromatography system (2-8% EtOAc/toluene in 20 min.) to afford the desired product as a colorless gum.

1. customthe reaction mixture was quenched with 5% aq. NaHCO3
2. extractionextracted with EtOAc
3. washThe combined organics were washed with 5% aq. NaHCO3, water and brine
4. dry with materialdried (Na2SO4)
5. concentrationconcentrated
6. customThe crude product was purified by Combi Flash chromatography system (2-8% EtOAc/toluene in 20 min.)