HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 22327376, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 20827740 | HCID 20827740 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 22327376 | HCID 22327376 | 29.3% |
Reaction Steps
Ethyl 3-chlorophenyl[2,4-diamino-6-(trifluoromethyl)phenyl]carbamate (80.2 mg) was dissolved in ethanol (1 ml), and to the solution was added sodium hydride (8.6 mg). The reaction mixture was heated at reflux for 2.5 hours. After allowing to cool, to the reaction mixture was added saturated aqueous sodium bicarbonate solution, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo. The resultant residue was purified by preparative TLC (2 mm, 20×20 cm, CHCl3-methanol=10:1) to give the title compound (20.6 mg, 29%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06939887B2 |
| Source dataset | uspto-grants-2005_09 |
| ORD ID | ord-c9600149f492401cab3cd4381252f402 |
| Source note | uspto-grants-2005_09 |