反应详情

A mixture of 3-methoxy-2,2-dimethylpropionic acid 5-[[3-(2-acetoxyethoxy)-2-fluoro-5-methoxyphenyl]-(4-carbamimidoylphen ylamino)methyl]-2-pyrimidin-2-yl-2H-[1,2,4]triazol-3-yloxymethyl ester acetate (13 mg), triethylamine (0.0074 mL), carbonic acid 2-methylallyl ester 4-nitrophenyl ester (5.6 mg), and DMF (2 mL) was stirred for 3 days at room temperature. The resulting mixture was poured into ethyl acetate (100 mL) and water (30 mL). After shaking the mixture, the organic layer was collected, sequentially washed twice with water (30 mL) and with saturated aqueous sodium chloride solution (30 mL), and dried over anhydrous magnesium sulfate. The resulting mixture was filtered, and the filtrate obtained was concentrated under reduced pressure. The residue obtained was purified by NAM silica gel column chromatography (mixed solvent of methanol-ethyl acetate) to obtain the captioned compound (13 mg).

1. stirringAfter shaking the mixture
2. customthe organic layer was collected
3. washsequentially washed twice with water (30 mL) and with saturated aqueous sodium chloride solution (30 mL)
4. dry with materialdried over anhydrous magnesium sulfate
5. filtrationThe resulting mixture was filtered
6. customthe filtrate obtained
7. concentrationwas concentrated under reduced pressure
8. customThe residue obtained
9. customwas purified by NAM silica gel column chromatography (mixed solvent of methanol-ethyl acetate)