HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrogen Bromide → HCID 178482454, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrogen Bromide | HCID 260 | — |
| Reactant | Propionic Acid | HCID 1032 | — |
| Reactant | HCID 178493935 | HCID 178493935 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178482454 | HCID 178482454 | — |
Reaction Steps
To a solution of N-[6-(4-fluorobenzyl)-3-hydroxy-4-methoxy-5-oxo-5,6,7,8-tetrahydro-2,6-naphthyridin-1-yl]-N-methylmethanesulfonamide (0.0207 g, 0.506 mmol) in CH2Cl2 (6 mL) was added 30% by weight HBr in propionic acid (0.196 g HBr, 2.42 mmol). Alternatively, 30% HBr in acetic acid can be used. After 1.5 hours, the product mixture was evaporated and the residue partitioned between CHCl3 and 10% KHSO4. The organic extract was dried with Na2SO4, filtered, and concentrated under vacuum. The residual material was purified using reverse phase HPLC eluting with 5%-95% acetonitrile (0.1% TFA) in H2O (0.1% TFA) to afford the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07598264B2 |
| Source dataset | uspto-grants-2009_10 |
| ORD ID | ord-b6d3358595bf4a8d9d34b2dfd33ca914 |
| Source note | uspto-grants-2009_10 |