HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 68407704, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | N-(tert-Butoxycarbonyl)-1,2-phenylenediamine | HCID 676311 | — |
| Reactant | 4-(4-Methylpiperazin-1-yl)benzoic acid | HCID 736532 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 68407704 | HCID 68407704 | — |
Reaction Steps
4-(1-Methylpiperazin-4-yl)benzoic acid (250 mg, 1.13 mmol) and 1-(N-t-butoxycarbonylamino)-2-aminobenzene (Method 17, 331 mg, 1.59 mmol) were dissolved in DMF (3 ml). 4-(4,6-dimethoxy-1,3,5-triazinyl-2-yl)-4-methylmorpholinium chloride (Method 18, 313 mg, 1.13 mmol) was added and the resulting solution was stirred for 20 hours at ambient temperature. The solution was poured into water and extracted several times with ethyl acetate. The combined organic extracts were dried over magnesium sulfate and evaporated. The residue was purified by flash chromatography (eluting with 99:1→9:1 dichloromethane:methanol) to afford the title compound as a colourless gum which crystallised on trituration (240 mg, 52%); Mass Spectrum: M+H+ 411.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08247562B2 |
| Source dataset | uspto-grants-2012_08 |
| ORD ID | ord-7c0bd5cc1f1740a98d12a5ef92bb78b9 |
| Source note | uspto-grants-2012_08 |