反应详情

3-(R)-Amino-1-(1-aminoisoquinolin-7-ylmethyl)pyrrolidin-2-one trifluoroacetate (80 mg, 0.216 mmol) and diisopropylethylamine (140 mg, 1.08 mmol) are dissolved in acetonitrile (12 mL), and stirred at room temperature for 15 minutes before adding thieno[3,2-b]pyridine-2-sulfonyl chloride dropwise as a solution in acetonitrile (8 mL). The reaction mixture is left at room temperature overnight, water (4 mL) added, and the solution concentrated in vacuo to remove the acetonitrile (ca. 4 mL of solution). 75% Acetonitrile/water (4 mL) is added. and the product purified by reverse phase preparative HPLC with gradient elution 10-40% acetonitrile/water (0.1% trifluoroacetic acid). The product fractions are combined, the acetonitrile removed in vacuo, and the aqueous solution lyophilized to give the product as a white powder (52 mg, 0.092 mmol).

1. waitThe reaction mixture is left at room temperature overnight
2. concentrationthe solution concentrated in vacuo
3. customto remove the acetonitrile (ca. 4 mL of solution)
4. addition75% Acetonitrile/water (4 mL) is added
5. customand the product purified by reverse phase preparative HPLC with gradient elution 10-40% acetonitrile/water (0.1% trifluoroacetic acid)
6. customthe acetonitrile removed in vacuo