反应详情

Potassium trimethylsilonolate (29 mg, 0.182 mmol) was added to a solution of 8-cyclopropanesulfonyl-4,5-difluoro-6-(2-fluoro-4-iodo-phenyl)-6,8-dihydro-imidazo[4′,5′:3,4]benzo[1,2-d]oxazol-7-one (I-19a: 65 mg, 0.121 mmol) in THF (5 mL) and the resulting mixture was stirred at room temperature for 1 hour. The reaction was monitored by TLC (50% ethyl acetate in hexane). The reaction mixture was concentrated and the concentrate was dissolved in water, acidified with 2N HCl and extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous Na2SO4 and concentrated to afford the crude product. Purification by column chromatography on silica gel (25-35% ethyl acetate in hexane) afforded 18 mg of the product (29.5% yield).

1. concentrationThe reaction mixture was concentrated
2. dissolutionthe concentrate was dissolved in water
3. extractionextracted with ethyl acetate
4. washThe organic layer was washed with brine
5. dry with materialdried over anhydrous Na2SO4
6. concentrationconcentrated
7. customto afford the crude product
8. customPurification by column chromatography on silica gel (25-35% ethyl acetate in hexane)