HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrogen Bromide → HCID 68455069, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrogen Bromide | HCID 260 | — |
| Reactant | HCID 11848248 | HCID 11848248 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 68455069 | HCID 68455069 | — |
Reaction Steps
A mixture of tert-butyl 4-(6-(5-(cyclopropylcarbamoyl)-2-methylphenyl)phthalazin-1-yl)-5,6-dihydropyridine-1(2H)-carboxylate (100 mg, 206 μmol) (Method B) in 2 mL methanol was stirred at RT was treated with 1 mL HBr 48% in H2O. The mixture was stirred for 2 h from 0° C. to RT. The mixture was diluted with 20 mL dichloromethane, washed with 1N NaOH to pH11. The mixture was extracted with dichloromethane (3×20 mL). The combined organics were washed with 20 mL brine, dried over anhydrous Na2SO4, concentrated via vacuum and purified by silica gel chromatography eluting with 10% 2M ammonia methanol/dichloromethane to give the title compound as a pale yellow solid. Found MS (ES+): 385(M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07759337B2 |
| Source dataset | uspto-grants-2010_07 |
| ORD ID | ord-395642e9898941d78f185fe8c1f76125 |
| Source note | uspto-grants-2010_07 |