HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → N-(4-Fluoro-3-chloro-phenyl)-2-[N-methyl-N-(2,2-difluoroethyl)-amino]-4-methylamino-5-nitro-benzoic acid amide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 2,2-difluoro-N-methylethanamine | HCID 23323250 | — |
| Reactant | N-(4-Fluoro-3-chloro-phenyl)-2-fluoro-4-methylamino-5-nitro-benzoic acid amide | HCID 67957648 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | N-(4-Fluoro-3-chloro-phenyl)-2-[N-methyl-N-(2,2-difluoroethyl)-amino]-4-methylamino-5-nitro-benzoic acid amide | HCID 86666463 | — |
Reaction Steps
A mixture of N-(2,2-difluoroethyl)-N-methyl-amine×HCl (64 mg, 0.48 mmol), DIPEA (0.64 ml, 3.73 mmol), N-(4-fluoro-3-chloro-phenyl)-2-fluoro-4-methylamino-5-nitro-benzoic acid amide (150 mg, 0.44 mmol) and MeCN (5 mL) is stirred for two weeks at reflux. Then the mixture is concentrated, diluted with EtOAc, washed with water, dried with Na2SO4 and concentrated and directly used in the next step.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08674113B2 |
| Source dataset | uspto-grants-2014_03 |
| ORD ID | ord-95e76a4fbdac4df9a635710c329bcbf1 |
| Source note | uspto-grants-2014_03 |