HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → N-(2-(tert-butylamino)pyridin-3-yl)-2,3-difluorobenzamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 2,3-Difluorobenzoyl chloride | HCID 519549 | — |
| Reactant | HCID 15656135 | HCID 15656135 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | N-(2-(tert-butylamino)pyridin-3-yl)-2,3-difluorobenzamide | HCID 59003070 | — |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
To a solution of N2-tert-butylpyridine-2,3-diamine in dry DCM (150 mL) was added DIEA (17 mL, 95.5 mmol). The solution was cooled to 0° C. and carefully added 2,3-difluorobenzoyl chloride (8.35 g, 47.30 mmol). The reaction was allowed to warm up to RT and stirred for 1 hr. The mixture was then washed with water, saturated NaHCO3, and dried over MgSO4. Removal of the solvent by evaporation, the residue was purified by silica gel chromatography (5%-60% EtOAc/hexane) to yield N-(2-(tert-butylamino)pyridin-3-yl)-2,3-difluorobenzamide (4.0 g, 13.10 mmol); LC-MS m/e=306.1 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07872031B2 |
| Source dataset | uspto-grants-2011_01 |
| ORD ID | ord-ef7d54834db9401fa8d9e04131ed7fd6 |
| Source note | uspto-grants-2011_01 |