反应详情

温度

37.5 °C

1.15 g (8.94 mmol) of Na2SO3 and 1.70 g (9.60 mmol) of Na2HPO4 hydrate were dissolved in 13 ml water. An ethanolic solution of 2.40 g (4.63 mmol) of 3-[5-(tetrahydro-pyran-4-yl)-1,3-dihydro-isoindole-2-carbonyl]-4-((S)-2,2,2-trifluoro-1-methyl-ethoxy)-benzenesulfonyl chloride was added. The reaction mixture was stirred at 35 to 40° C. during 1 hour and then overnight at room temperature. 1.3 g Speedex was added, the reaction mixture was filtered and the filtrate was evaporated. The crude product was treated with aqueous citric acid/NaCl solution then extracted with MTBE/THF 1:1. The organic solvent was evaporated and the residue was dissolved in MeOH/water (2:1), and treated with 800 mg (9.52 mmol) of NaHCO3. 1 g Speedex was added and the reaction mixture was filtrated and concentrated in vacuo. The residue was purified chromatographically by using a reverse phase column (RP-18, water/methanol) to provide 1.12 g (48%) of the title compound as a white foam. MS (m/e): 484.3 [M+H]+.

1. customovernight
2. customat room temperature
3. addition1.3 g Speedex was added
4. filtrationthe reaction mixture was filtered
5. customthe filtrate was evaporated
6. additionThe crude product was treated with aqueous citric acid/NaCl solution
7. extractionthen extracted with MTBE/THF 1:1
8. customThe organic solvent was evaporated
9. dissolutionthe residue was dissolved in MeOH/water (2:1)
10. addition1 g Speedex was added
11. filtrationthe reaction mixture was filtrated
12. concentrationconcentrated in vacuo
13. customThe residue was purified chromatographically