反应详情

A solution of oxalyl chloride (4.0 mL, 46 mmol) in CH2Cl2 (100 mL) at −78° C. was added DMSO (6.5 mL, 92 mmol) dropwise. The mixture was stirred for 10 minutes after which the title compound from Example 13.2 (7.92 mg, 41.6 mmol) in CH2Cl2 (30 mL) was added dropwise. The mixture was stirred for an additional 30 minutes and Et3N (2.9 mL, 208 mmol) was added dropwise. The reaction was then allowed to warm to room temperature. Water (150 mL) was then added and the organic layer was washed with brine, dried over sodium sulfate, filtered and concentrated. The crude product was purified by column chromatography (10-20% EtOAc/hexanes) to yield the title compound as an orange oil (4.98 g, 64%).

1. additionwas added dropwise
2. washthe organic layer was washed with brine
3. dry with materialdried over sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated
6. customThe crude product was purified by column chromatography (10-20% EtOAc/hexanes)