HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 1-Chloro-4-((3-chloro-4-methoxybenzyl)amino)-6-phthalazinecarbonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 3-Chloro-4-methoxybenzylamine | HCID 738038 | — |
| Reactant | 1,4-Dichlorophthalazine-6-carbonitrile | HCID 10656738 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 1-Chloro-4-((3-chloro-4-methoxybenzyl)amino)-6-phthalazinecarbonitrile | HCID 10451065 | 55.6% |
Reaction Steps
66.2 g of 6-cyano-1,4-dichlorophthalazine and 92 g of 3-chloro-4-methoxybenzylamine were suspended in 1,200 ml of tetrahydrofuran. After adding 250 ml of triethylamine, the resulting mixture was heated under reflux for 6 hours. The resulting crystals were filtered off and the filtrate was evaporated. The residue was purified by silica gel column chromatography (toluene:tetrahydrofuran=10:1) to give 59 g of 1-chloro-4-(3-chloro-4-methoxybenzyl)amino-6-cyanophthalazine as pale yellow crystals. M.p.: 213.0-214.5° C., Mass 359(MH+),
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06288064B1 |
| Source dataset | uspto-grants-2001_09 |
| ORD ID | ord-62ae323658834ab08d0c501162fe7741 |
| Source note | uspto-grants-2001_09 |