HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cesium carbonate → HCID 67317949, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 1-Chloro-4-phenylphthalazine | HCID 272109 | — |
| Reactant | 2,4-Dimethoxybenzylamine hydrochloride | HCID 3084343 | — |
| Solvent | tert-Butanol | HCID 6386 | — |
| Product | HCID 67317949 | HCID 67317949 | — |
Reaction Steps
In a nitrogen purged 75 mL sealed tube, dissolved 2,4-dimethoxybenzylamine hydrochloride (2.54 g, 12.5 mmol), cesium carbonate (4.06 g, 12.5 mmol) in tBuOH (15 mL). Added 1-chloro-4-phenylphthalazine (2.0 g, 8.31 mmol) and the tube was stirred at 100° C. for 17 h. The tube was cooled to RT, and the mixture was concentrated in vacuo. Dissolved the crude material in DCM, and filtered the solution to remove cesium carbonate. Performed silica gel chromatography using 0-100% EtOAc/Hex and concentrated to yield N-(2,4-dimethoxybenzyl)-4-phenylphthalazin-1-amine as orange oil. MS [M+H]=372; Calc'd 371.4 for C23H21N3O2.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08557816B2 |
| Source dataset | uspto-grants-2013_10 |
| ORD ID | ord-fdec92ae05d54db6987dab5869e13fa5 |
| Source note | uspto-grants-2013_10 |