HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Carbonate → Methyl 2-chloro-3-hydroxyiminomethyl-4-methylsulfonylbenzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Hydroxylamine HCl | HCID 21645 | — |
| Reactant | Methyl 2-chloro-3-formyl-4-methylsulfonylbenzoate | HCID 18517410 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Product | Methyl 2-chloro-3-hydroxyiminomethyl-4-methylsulfonylbenzoate | HCID 86584467 | 96.6% |
Reaction Steps
55.23 g (0.199 mol) of methyl 2-chloro-3-formyl-4-methylsulfonylbenzoate are suspended in 400 ml of methanol/100 ml of water and treated with 15.27 g (0.219 mol) of hydroxylammonium chloride. 11.56 g (0.11 mol) of sodium carbonate—dissolved in 100 ml of water—are then slowly added dropwise at room temperature. After stirring at room temperature for 4 hours, the methanol is removed in a rotary evaporator, the residue is diluted with water and the mixture is extracted three times with dichlormethane. 56.05 g (96% of theory) of methyl 2-chloro-3 hydroximinomethyl-4-methylsulfonylbenzoate having a melting point of 126-130° C. are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06211216B1 |
| Source dataset | uspto-grants-2001_04 |
| ORD ID | ord-0d46fc7f029142a692be586fe3a9b785 |
| Source note | uspto-grants-2001_04 |