HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 14720326, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | N-(2,4-Difluorophenyl)-4-pyridinemethanamine | HCID 14720325 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 14720326 | HCID 14720326 | — |
Reaction Steps
A 4.7 g. portion of 4-(2,4-difluorophenylaminomethyl)pyridine was dissolved in 15 ml. of chloroform, and 4.1 g. of potassium carbonate was added, followed by 2.3 ml. of methanesulfonyl chloride. The mixture was stirred under reflux overnight, and then for several days at ambient temperature. It was then diluted with 20 ml. of dichloromethane and 20 ml. of aqueous sodium bicarbonate, and 5 ml. of 2N sodium hydroxide was added. The organic phase was then washed with aqueous sodium bicarbonate, dried and evaporated. The residue was dissolved in dichloromethane and chromatographed over silica gel, to obtain 0.5 g. of impure product, which was triturated with diethyl ether to obtain 0.29 g. of the desired product, m.p. 101°-105°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04874775 |
| Source dataset | uspto-grants-1989_10 |
| ORD ID | ord-11afd315273f48078ffc5ac7aef89735 |
| Source note | uspto-grants-1989_10 |