HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → HCID 178448116, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Phthalazine | HCID 9207 | — |
| Reactant | HCID 178448118 | HCID 178448118 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 178448116 | HCID 178448116 | — |
Reaction Steps
trans 1-(4-isoproryl-cyclohexylamino)-4-[2-methoxy-pyridin-4-yl)-methyl]-phthalazine: Under N2 atmosphere, in an ampoule 1.73 g (12 mMol) of trans 4-isopropyl-cyclohexylamine (preparation see Arzneim. Forsch. 1969, 19,140) and 700 mg (2.4 mMol) of 1-chloro-4-[2-methoxy-pyridin-4-yl)methyl]phthalazine are heated during 17 h at 140° C. The reaction mixture is suspended in EtOAc, and 1.5 ml of NH3 solution (25%) and water are added. The isolated aqueous phase is extracted another two times with EtOAc, and the organic phases are washed with water and brine, dried (Na2SO4) and evaporated to dryness. Column chromatography (SiO2; hexane/EtOAc 1:1) results in the title compound: M.p. 65-66° C.; FAB-MS: (M+H)+=391.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07399761B2 |
| Source dataset | uspto-grants-2008_07 |
| ORD ID | ord-c6f6954f88d54203b5aac40efa587971 |
| Source note | uspto-grants-2008_07 |