反应详情

To a solution of 3C (305 mg, 1.458 mmol) and pyridine (0.7 mL) in CH3CN (30 mL) cooled to 0° C. was added bezenesulfonyl chloride (274 mg, 1.550 mmol). After addition, the reaction mixture was stirred at RT for 1 hour, then concentrated under reduced pressure. The resultant residue was dissolved in CH2Cl2 (100 mL), washed with water (2×50 mL), saturated NaCl (50 mL). The organic layer was dried (MgSO4), filtered and concentrated. The residue was purified by silica gel column chromatography eluting with 2% of 2 M NH3 in MeOH/CH2Cl2 to give the title compound as a light brown solid (200 mg, 40% yield). LC/MS (method A): retention time=2.78 min, (M+H)+=351.

1. additionAfter addition
2. concentrationconcentrated under reduced pressure
3. dissolutionThe resultant residue was dissolved in CH2Cl2 (100 mL)
4. washwashed with water (2×50 mL), saturated NaCl (50 mL)
5. dry with materialThe organic layer was dried (MgSO4)
6. filtrationfiltered
7. concentrationconcentrated
8. customThe residue was purified by silica gel column chromatography
9. washeluting with 2% of 2 M NH3 in MeOH/CH2Cl2