反应详情

Phosphoric acid di-tert-butyl ester 4-{4-[(2,6-dichloro-benzoylamino)-methyl]-phenyl}-2-oxo-2H-pyridin-1-ylmethyl ester from the previous step was dissolved in 20 mL acetonitrile, 20 mL acetic acid and 20 mL water, and heated at 70° C. for four hours. All volatile components were evaporated under vacuum and the residue was dissolved in 10 mL DMF. Slow addition of acetonitrile (˜60 mL) precipitated the product which was filtered, washed with more acetonitrile and dried, giving phosphoric acid mono-(4-{4-[(2,6-dichloro-benzoylamino)-methyl]-phenyl}-2-oxo-2H-pyridin-1-ylmethyl)ester (1.17 g, 56% over three steps) as a white powder.

1. customAll volatile components were evaporated under vacuum
2. dissolutionthe residue was dissolved in 10 mL DMF
3. additionaddition of acetonitrile (˜60 mL)
4. customprecipitated the product which
5. filtrationwas filtered
6. washwashed with more acetonitrile
7. customdried