HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Benzylpiperazine → 6-(4-BENZYLPIPERAZIN-1-YL)PYRIDAZINE-3-CARBOXYLIC Acid (3-METHYLBUTYL)AMIDE
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Benzylpiperazine | HCID 75994 | — |
| Reactant | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Reactant | 6-chloro-N-(3-methylbutyl)pyridazine-3-carboxamide | HCID 16733786 | — |
| Catalyst | Tetrabutylammonium Bromide | HCID 74236 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 6-(4-BENZYLPIPERAZIN-1-YL)PYRIDAZINE-3-CARBOXYLIC Acid (3-METHYLBUTYL)AMIDE | HCID 86597216 | 75.2% |
Reaction Steps
A stirred mixture of 6-chloropyridazine-3-carboxylic acid (3-methylbutyl)amide (0.113 g, 0.5 mmol), 1-benzylpiperazine (90 mg, 0.5 mmol), tetrabutylammonium bromide (27 mg, 0.084 mmol) and 1,8-diazabicylco[5.4.0]undec-7-ene (152 mg, 1.0 mmol) was heated under reflux in dioxane (10 mL) overnight. The solvent was evaporated. Residue was treated with 2% methanol in water (25 mL). The solid, which precipitated, was filtered off and dried in vacuo to give 138 mg (0.376 mmol) of the title compound in 75% yield. 1H NMR (300 MHz, CDCl3) δ 7.98, 7.87, 7.36-7.32, 6.94, 3.76-3.74, 3.57, 3.50-3.46, 2.60-2.58, 1.74-1.68, 1.52-1.48, 0.94. MS (ES+) m/z 368.2 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07964591B2 |
| Source dataset | uspto-grants-2011_06 |
| ORD ID | ord-bcfefd340aab440b8f114ed91c0bee57 |
| Source note | uspto-grants-2011_06 |