HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 68981429, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Methoxyacetyl chloride | HCID 96623 | — |
| Reactant | HCID 21106565 | HCID 21106565 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 68981429 | HCID 68981429 | 76% |
Reaction Steps
4-Bromo-2-isopropyl-7-methylamino-2H-phthalazin-1-one (0.5 g, 1.69 mmol) was dissolved in DMF (5 ml). To this was added NaH (60%, 0.19 g, 5.1 mmol) as a suspension in DMF (2 ml). The mixture was stirred at RT for 30 min then methoxyacetyl chloride (0.27 g, 2.5 mmol) was added dropwise and the reaction mixture was stirred at RT for 24 hours. After this time, water (10 ml) was added cautiously, the mixture was extracted with EtOAc (3×10 ml), the organic layers were combined, dried (MgSO4), filtered and concentrated under vacuum. Flash column chromatography (elution: 50% hexane, 50% EtOAc) gave the title compound (0.47 g, 76% yield) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07501410B2 |
| Source dataset | uspto-grants-2009_03 |
| ORD ID | ord-49332a5f9c03447d85bbd807a0c7d77e |
| Source note | uspto-grants-2009_03 |