反应详情

Dissolve {1-[1-(4-fluoro-2-{2-[5-fluoro-2-(2-[1,2,3]triazol-1-yl-ethylamino)-pyrimidin-4-yl]-benzo[b]thiophen-7-yl}-phenyl)-ethylcarbamoyl]-ethyl}-carbamic acid 9H-fluoren-9-ylmethyl ester (129 mg, 167 μmol) in piperidine (5 mL). Stir the mixture at RT for 30 min and then dilute with chloroform/IPA (3/1, 100 mL). Wash the organic phase with water/aqueous saturated sodium chloride, dry over sodium sulfate, and concentrate in vacuo. Purify the crude product by FCC (10% methanol in DCM to chloroform/methanol/ammonium hydroxide (7/3/0.05) as a gradient to give the title compound as a yellow solid (72 mg, 78%). MS (ES) m/z 549 [M+1]+.

1. washWash the organic phase with water/aqueous saturated sodium chloride
2. dry with materialdry over sodium sulfate
3. concentrationconcentrate in vacuo
4. customPurify the crude product by FCC (10% methanol in DCM to chloroform/methanol/ammonium hydroxide (7/3/0.05) as a gradient