HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzoic acid, 3-(chlorosulfonyl)- → 3-{[Ethylamino-(4-ethyl-4,5-dihydro-pyrazol-1-yl)-methylene]-sulfamoyl}-benzoic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzoic acid, 3-(chlorosulfonyl)- | HCID 77641 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 178464602 | HCID 178464602 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 3-{[Ethylamino-(4-ethyl-4,5-dihydro-pyrazol-1-yl)-methylene]-sulfamoyl}-benzoic acid | HCID 178464649 | 4% |
Reaction Steps
Under N2 atmosphere, 1.0 g 4,N-diethyl-4,5-dihydro-pyrazole-1-carboxamidine was dissolved in 15 mL dry DCM, and 1.14 mL DiPEA and 1.31 g of 3-(chlorosulfonyl)benzoic acid were added. The mixture was stirred overnight at room temperature and evaporated to dryness. The residue was purified by flash chromatography (first column with DCM/MeOH/acetic acid 84:15:1; second column with DCM/MeOH/NH4OH 84:15:1) to yield 0.08 g (4%) of an off-white powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08901108B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-cd6963d235904710a60e3e06d944243a |
| Source note | uspto-grants-2014_12 |