HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,4-Dichloro-5,6,7,8-tetrahydro-5,8-ethanophthalazine → HCID 87292593, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,4-Dichloro-5,6,7,8-tetrahydro-5,8-ethanophthalazine | HCID 6416107 | — |
| Reactant | HCID 178461828 | HCID 178461828 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 87292593 | HCID 87292593 | — |
Reaction Steps
A solution of 1,4-dichloro-5,6,7,8-tetrahydro-5,8-ethanophthalazine (Alfa Aesar) (0.109 g, 0.474 mmol), iPr2Zn (1 M in toluene, 0.50 mL, 0.50 mmol), PdCl2dppf CH2Cl2 (19.3 mg, 0.024 mmol) in dioxane (1.5 mL) was stirred at 80° C. for 2.5 hours, quenched with 1 N HCl, diluted with EtOAc, washed with saturated aqueous NaHCO3 and brine, dried (Na2SO4), and filtered. The residue was chromatographed on SiO2 (10% Et2O/CH2Cl2 to 5% MeOH/CH2Cl2) to give impure title compound as a tacky solid (34.9 mg). LC/MS (APCI) M/Z 237.1 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08629143B2 |
| Source dataset | uspto-grants-2014_01 |
| ORD ID | ord-6e02ca35a2c040e69f878abdeb1a1e16 |
| Source note | uspto-grants-2014_01 |