HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 90022747, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 2-Chloro-6-fluorobenzylamine | HCID 84833 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 64280908 | HCID 64280908 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 90022747 | HCID 90022747 | 6% |
Reaction Steps
A solution of 4-Chloro-N-(3,4-dimethoxyphenyl)pyridine-3-sulfonamide (IntD1) (0.5 g, 1.50 mmol), 2-chloro-6-fluoro-benzylamine (0.26 g, 1.67 mmol) and K2CO3 (0.41 g, 3.0 mmol) in DMF (10 mL) was heated at 130° C. for 4 h. The mixture was added to saturated aqueous NaHCO3 (50 mL), extracted with EtOAc (3×25 mL) and the combined organic phases dried over Na2SO4 and concentrated in vacuo. Purification by gradient column chromatography eluting with 0-45% EtOAc in hexane yielded the title compound (40 mg, 0.09 mmol).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09249160B2 |
| Source dataset | uspto-grants-2016_02 |
| ORD ID | ord-a0f86a5b90154379b85d43e00a9bb429 |
| Source note | uspto-grants-2016_02 |