HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → phosphoric acid mono-(4-{4-[(2,6-dichloro-benzoylamino)-methyl]phenyl}-2-oxo-2H-pyridin-1-ylmethyl)ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | phosphoric acid di-tert-butyl ester 4-{4-[(2,6-dichloro-benzoylamino)-methyl]-phenyl}-2-oxo-2H-pyridin-1-ylmethyl ester | HCID 71149943 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | phosphoric acid mono-(4-{4-[(2,6-dichloro-benzoylamino)-methyl]phenyl}-2-oxo-2H-pyridin-1-ylmethyl)ester | HCID 71149979 | 56% |
Reaction Steps
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.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09000015B2 |
| Source dataset | uspto-grants-2015_04 |
| ORD ID | ord-68496ee0d21c4111888b3e6a549017df |
| Source note | uspto-grants-2015_04 |