HuagongsheHuagongshe Chemistry Print Report · For research reference only
Oxalyl chloride → HCID 87955231, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Reactant | 2-Ethoxy-5-(4-methylpiperazine-1-sulfonyl)benzoic acid | HCID 12134865 | — |
| Catalyst | Dimethylformamide | HCID 6228 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 87955231 | HCID 87955231 | 84% |
Reaction Steps
Oxalyl chloride (11.7 ml, 134 mmol) was added dropwise to an ice cold suspension of 2-ethoxy-5-(4-methylpiperazin-1-ylsulphonyl)benzoic acid (EP 812845 A1) (20.0 g, 60.9 mmol) and dimethylformamide (2 drops) in dichloromethane (200 ml) over 15 minutes, and the reaction mixture stirred at room temperature for 18 hours. The mixture was concentrated under reduced pressure, the residue triturated with ether then ethyl acetate and dried at 40° C. for 16 hours, to afford the title compound, (19.6 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06407114B1 |
| Source dataset | uspto-grants-2002_06 |
| ORD ID | ord-87308cba657645fdbe8c21f0f9bc9a46 |
| Source note | uspto-grants-2002_06 |