HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 68676974, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | Methyl 3-amino-2,6-difluorobenzoate | HCID 45480188 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 68676974 | HCID 68676974 | — |
Reaction Steps
To a solution of methyl 3-amino-2,6-difluorobenzoate (530 mg, 2.83 mmol) and pyridine (0.28 mL, 3.40 mmol) in 10 mL CH2Cl2 was added methanesulfonyl chloride (0.24 mL, 3.11 mmol). After 24 h at room temperature, the reaction mixture was washed with saturated aqueous NaHCO3 and extracted with CHCl3 to provide crude methyl 2,6-difluoro-3-[(methylsulfonyl)amino]benzoate as a solid (ESI-MS 264 (M−H)), which was hydrolyzed using aqueous NaOH to provide 2,6-difluoro-3-[(methylsulfonyl)amino]benzoic acid (ESI-MS 250 (M−H)), which was used without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07645771B2 |
| Source dataset | uspto-grants-2010_01 |
| ORD ID | ord-6a05b3f058904232abb5da3f02b840ad |
| Source note | uspto-grants-2010_01 |