HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 69936757, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | 3-Aminopyridine | HCID 10009 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | HCID 67106993 | HCID 67106993 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 69936757 | HCID 69936757 | — |
Reaction Steps
HOBT (102 mg, 0.67 mmol) was added in one charge to a stirred solution of 5-[(dimethylamino)carbonyl]-2-[(phenylmethyl)oxy]benzoic acid (may be prepared as described in Description 59; 200 mg, 0.67 mmol), 3-pyridinamine (62.9 mg, 0.67 mmol) and EDC (128 mg, 0.67 mmol) in N,N-dimethylformamide (5 ml) under nitrogen at room temperature. The reaction mixture was stirred at room temperature for 4 h. The mixture was diluted with water (50 ml). The precipitate was collected by filtration. The solid was dissolved in ethyl acetate (100 ml), and the organic phase was washed with NaOH (1 mol/l 25 ml), water (25 ml), saturated brine (25 ml), dried over sodium sulfate, and evaporated in vacuo to yield the title compound as a white solid. 78 mg.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08778939B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-9d148bd02f994cab8908feea5236dd69 |
| Source note | uspto-grants-2014_07 |