HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium borohydride → 2-chloro-5-(hydroxymethyl)Benzenesulfonamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium borohydride | HCID 4148881 | — |
| Reactant | Benzoic acid, 3-(aminosulfonyl)-4-chloro-, ethyl ester | HCID 15938945 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 2-chloro-5-(hydroxymethyl)Benzenesulfonamide | HCID 18374381 | 88.9% |
Reaction Conditions
| Temperature | 4 °C |
|---|
Reaction Steps
To a solution of 4-chloro-3-sulfamoyl-benzoic acid ethyl ester (46.95 g, 166 mmol) in 500 mL of dry tetrahydrofuran is added dropwise, with stirring, 199 mL of a 2 M solution of lithium borohydride in tetrahydrofuran. The mixture is stirred and refluxed for 5 hr, then left at room temperature for 18 h, and is then carefully diluted with 400 mL of water. The mixture is cooled to 4° C. for 24 hours and filtered to yield 32.7 g (82%) of the title compound as an off-white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08975439B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-c766ae50283741528b136080269164fd |
| Source note | uspto-grants-2015_03 |