HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 178513591, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 178524163 | HCID 178524163 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178513591 | HCID 178513591 | 49.3% |
Reaction Steps
To a mixture of 2-[4-(2,6-difluoro-benzoylamino)-1H-pyrazol-3-yl]-1H-benzimidazole-5-carboxylic acid (100 mg, 0.26 mmol), EDC (75 mg, 0.39 mmol) and HOBt (53 mg, 0.39 mmol) in DMF (1.5 ml) was successively added diisopropylethylamine (0.15 ml, 1.04 mmol) and ammonium chloride (28 mg, 0.52 mmol). The mixture was stirred at ambient temperature for 48 h and then reduced in vacuo. Water was added and the precipitate formed collected by filtration and dried through azeotrope with toluene to afford 2-[4-(2,6-difluoro-benzoylamino)-1H-pyrazol-3-yl]-1H-benzimidazole-5-carboxylic acid amide (49 mg, 49%) as a beige solid. (LC/MS: Rt 2.54, [M+H]+ 382.99).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07977477B2 |
| Source dataset | uspto-grants-2011_07 |
| ORD ID | ord-e5c622c47e384de2b529789c4f2bbafe |
| Source note | uspto-grants-2011_07 |