HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 67107332, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | 1H-pyrazol-4-amine | HCID 78035 | — |
| Reactant | 2-(Benzyloxy)-5-(pyridin-4-yl)benzoic acid | HCID 66990482 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 67107332 | HCID 67107332 | — |
Reaction Steps
Neat 1H-pyrazol-4-amine (49.0 mg, 0.59 mmol) was added in one charge to a stirred solution of 2-[(phenylmethyl)oxy]-5-(4-pyridinyl)benzoic acid (may be prepared as described in Description 79; 150 mg, 0.49 mmol), EDC (283 mg, 1.47 mmol) and HOBT (226 mg, 1.47 mmol) in dimethylformamide (4 ml) in air at room temperature. The reaction mixture was stirred at room temperature overnight. 30 ml water was added, and the mixture was extracted with ethyl acetate (70 ml×2). The organic layers were combined, dried over MgSO4, and concentrated in vacuo. The residue was further purified by pre-HPLC (Gilson GX-281; Shimadzu 15 μm 250*20 mm; A: 10 mMol NH4HCO3/Water; B: CH3CN) to yield the title compound as a white solid. 50 mg.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08778939B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-f8e20d1440a54050aaf06939cde31582 |
| Source note | uspto-grants-2014_07 |