反应详情

Triethylamine (0.35 mL, 2.5 mmol) is added dropwise to a solution of 5-pyridin-3-yl-thiophene-2-sulfonyl chloride (0.22 g, 0.85 mmol) and 3-(S)-amino-1-(1-chloro-isoquinolin-7-ylmethyl)-pyrrolidin-2-one hydrochloride (0.22 g, 0.71 mmol) in CH3CN (5 mL). The suspension is stirred at room temperature overnight then concentrated to dryness. The residue is diluted with methylene chloride and washed with saturated NaHCO3 solution and brine. The organic layer is dried over MgSO4, filtered, concentrated, and then purified by column chromatography eluting with a gradient of 1% MeOH/CH2Cl2 to 5% MeOH/CH2Cl2 to give the product (0.23 g, 0.45 mmol) as a white solid.

1. concentrationthen concentrated to dryness
2. additionThe residue is diluted with methylene chloride
3. washwashed with saturated NaHCO3 solution and brine
4. dry with materialThe organic layer is dried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated
7. custompurified by column chromatography
8. washeluting with a gradient of 1% MeOH/CH2Cl2 to 5% MeOH/CH2Cl2