HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 67345696, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 4-Fluorophenyl isocyanate | HCID 70955 | — |
| Reactant | HCID 58379032 | HCID 58379032 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67345696 | HCID 67345696 | 97.7% |
Reaction Steps
Treat a solution of (R)-(4-(4-(4-fluorophenyl)phthalazin-1-yl)piperazin-2-yl)-methanol (0.15 g, 0.44 mmol) in CH2Cl2 (3 ml) with 1-fluoro-4-isocyanatobenzene (0.04 g, 0.31 mmol). Stir the reaction at ambient temperature for 30 min and then concentrate the reaction mixture. Purify the resulting residue by flash silica gel chromatography (0-50% EtOAc in hexanes, then switch to 3% MeOH in CH2Cl2) to yield a solid. Dissolve the solid in MeOH (1 mL) and treat with 1 N aqueous HCl (0.13 mL, 0.13 mmol). Concentrate the solution to obtain the title compound as a solid (0.065 g, 29%). ES/MS m/z 476.0 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08404687B2 |
| Source dataset | uspto-grants-2013_03 |
| ORD ID | ord-8fd715f719b841aa837b6f85fb5ca3b3 |
| Source note | uspto-grants-2013_03 |