HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → HCID 22741970, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | 4'-Amino-2'-hydroxyacetophenone | HCID 459296 | — |
| Reactant | 1-Chloro-4-(4-pyridinylmethyl)phthalazine | HCID 1944609 | — |
| Solvent | 1,3-Dimethyl-2-imidazolidinone | HCID 6661 | — |
| Product | HCID 22741970 | HCID 22741970 | — |
Reaction Steps
302 mg (2.0 mmol) 2-acetyl-5-aminophenol (Maybridge) and 256 mg (1.00 mmol) 1-chloro-4-(4-pyridylmethyl)phthalazine (Example 67A.1) in 2 ml DMEU are heated for 3-18 h to 100° C. The reaction mixture is stirred with 10 ml NH3 solution (10% in water) and 25 ml ethyl actetate (or dichloromethane) and filtered via Celite. The organic phase of the filtrate is dried (Na2SO4), evaporated, and chromatographed (SiO2; ethyl acetate/CH3OH, 40:1→10:1) Crystallization from acetonitrile yields the title compound: m.p.: 234-236° C.; HPLC: tRet(Grad5-40)=9.5; FAB MS (M+H)+=371.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06514974B2 |
| Source dataset | uspto-grants-2003_02 |
| ORD ID | ord-8a17cefe45b941139273a43df82c328e |
| Source note | uspto-grants-2003_02 |