HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Methoxybenzylamine → HCID 58447313, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Methoxybenzylamine | HCID 75452 | — |
| Reactant | Binap, (A+-)- | HCID 634876 | — |
| Reactant | 6-Bromophthalazin-1(2h)-one | HCID 11535918 | — |
| Reactant | Sodium t-butoxide | HCID 23676156 | — |
| Catalyst | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 58447313 | HCID 58447313 | 35.5% |
Reaction Steps
A mixture of 6-bromo-2H-phthalazin-1-one (50 mg, 0.22 mmol), 4-methoxybenzylamine (0.030 mL, 0.24 mmol), Pd2(dba)3 (20 mg, 0.022 mmol), rac-BINAP (41 mg, 0.066 mmol) and NaOt-Bu (52 mg, 0.55 mmol) in toluene (10 mL) was heated at reflux for 3 h. The mixture was allowed to cool, diluted with EtOAc (25 mL) and washed with NaHCO3 (25 mL). The organic layer was dried over anhydrous sodium sulfate and concentrated. Chromatography on silica (EtOAc/hexanes) yielded the title compound (22 mg, 35%). 1H-NMR (DMSO-d6) δ: 12.1 (s, 1H), 8.05 (s, 1H), 7.88 (d, 1H), 7.30 (m, 3H), 7.10 (dd, 1H), 6.90 (d, 2H), 6.75 (s, 1H), 4.20 (d, 2H), 3.85 (s, 3H); m/z (M+1)=282.22.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08044041B2 |
| Source dataset | uspto-grants-2011_10 |
| ORD ID | ord-8feb20dbef1247a78172db24c93cd76e |
| Source note | uspto-grants-2011_10 |