反应详情

The mixture obtained in Example 26 (˜2.5 g total) was dissolved in dichloromethane (30 mL). Oxalyl chloride (2 M in dichloromethane, 16.3 mL. 32.6 mmol) was added and the reaction was stirred for 30 min. The reaction was quenched with methanol, then diluted with dichloromethane and washed with water. The organic phase was dried over anhydrous magnesium sulfate, filtered and concentrated, then chromatographed in 20-50% ethyl acetate in hexanes to yield the title product 1.55 g, 26% (2 steps).

1. customThe reaction was quenched with methanol
2. additiondiluted with dichloromethane
3. washwashed with water
4. dry with materialThe organic phase was dried over anhydrous magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated
7. customchromatographed in 20-50% ethyl acetate in hexanes