HuagongsheHuagongshe Chemistry Print Report · For research reference only
(3,5-Dimethoxyphenyl)methanamine → HCID 24948720, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | (3,5-Dimethoxyphenyl)methanamine | HCID 420973 | — |
| Reactant | Binap, (A+-)- | HCID 634876 | — |
| 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 24948720 | HCID 24948720 | 2.1% |
Reaction Steps
A mixture 6-bromo-4-chloro-2H-phthalazin-1-one (105 mg, 0.405 mmol), 3,5-dimethoxybenzylamine (0.64 mL, 0.424 mmol), Pd2(dba)3 (25 mg, 0.027 mmol), rac-BINAP (78 mg, 0.125 mmol) and NaOt-Bu (92 mg, 0.963 mmol) in DMA (6 mL) was heated at 80° C. for 45 minutes. 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-(3,5-dimethoxy-benzylamino)-2H-phthalazin-1-one (3 mg) as a brown solid, 1H (400 MHz, CDCl3) δ: 3.65 (d, 6H), 4.28 (s, 2H), 6.25 (m, 1H), 6.42 (m, 2H), 6.81 (m, 1H), 6.95 (m, 2H), 8.00 (m, 1H), ppm. m/z (M+1) 345.92.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08349836B2 |
| Source dataset | uspto-grants-2013_01 |
| ORD ID | ord-243fbb483c874771878f6c63a5f97d88 |
| Source note | uspto-grants-2013_01 |