反应详情

To 11a (219 mg, 0.67 mmol) in CH2Cl2 (30 mL) was added oxalyl chloride (0.07 mL, 0.80 mmol) and a drop of DMF. The mixture was then concentrated, and the residue was redissolved in CH2Cl2 and divided into 5 portions. To one portion, dimethylamine (2.0M, 0.3 mL, 0.54 mmol) was added, and the mixture was stirred at room temperature until no SM was observed by LCMS analysis. The reaction was concentrated and purified by preparative HPLC to give the desired product, 11b.

1. concentrationThe mixture was then concentrated
2. dissolutionthe residue was redissolved in CH2Cl2
3. concentrationThe reaction was concentrated
4. custompurified by preparative HPLC