HuagongsheHuagongshe Chemistry Print Report · For research reference only
Binap, (A+-)- → HCID 58447338, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Binap, (A+-)- | HCID 634876 | — |
| Reactant | 3-(Difluoromethoxy)benzylamine | HCID 2063350 | — |
| Reactant | Sodium t-butoxide | HCID 23676156 | — |
| Reactant | 6-Bromo-4-chlorophthalazin-1(2H)-one | HCID 53308487 | — |
| Catalyst | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Solvent | Dimethylacetamide | HCID 31374 | — |
| Product | HCID 58447338 | HCID 58447338 | 8.4% |
Reaction Steps
A mixture 6-bromo-4-chloro-2H-phthalazin-1-one (150 mg, 0.578 mmol), 3-(difluoromethoxy)benzylamine (0.074 mL, 0.645 mmol), Pd2(dba)3 (48 mg, 0.052 mmol), rac-BINAP (108 mg, 0.173 mmol) and NaOtBu (139 mg, 1.445 mmol) in DMA (6 mL) was heated at 80° C. for 1.5 h. The mixture was allowed to cool, diluted with EtOAc and washed with water. The organic layer was washed with sat.aq. NaHCO3, brine and dried (Na2SO4). Chromatography on silica (EtOAc/hexanes) afforded 4-chloro-6-(3-difluoromethoxy-benzylamino)-2H-phthalazin-1-one (17 mg) as an off white solid, 1H (400 MHz, CDCl3) δ: 4.32 (s, 2H), 6.36 (t, 1H), 6.77 (d, 1H), 6.90 (t, 2H), 6.99 (s, 1H), 7.08 (d, 1H), 7.21 (t, 1H), 8.00 (d, 1H), 10.15 (s, 1H) ppm; m/z (M+1) 351.92.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08349836B2 |
| Source dataset | uspto-grants-2013_01 |
| ORD ID | ord-26b780aecc60442fa1434e0d01da8163 |
| Source note | uspto-grants-2013_01 |