HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl 4-sulphamoylbenzoate → 4-(Hydroxymethyl)benzenesulfonamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl 4-sulphamoylbenzoate | HCID 89847 | — |
| Reactant | Lithium borohydride | HCID 4148881 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 4-(Hydroxymethyl)benzenesulfonamide | HCID 10081162 | 17% |
Reaction Steps
To a solution of 5.2 g 4-sulfamoyl-benzoic acid methyl ester in 100 mL THF and 1.44 mL MeOH, 0.77 g lithium borohydride was added portion-wise over a period of 10 minutes. The mixture was heated at reflux overnight, cooled to room temperature, and poured onto ice containing 100 mL 1N HCl. The mixture was extracted with EtOAc, and the organic layer was dried over MgSO4 and concentrated under reduced pressure. The residue was purified by automated flash chromatography (EtOAc/Hexane 1:1) to give 0.75 gram (17%) of product. 1H NMR (400 MHz, DMSO-d6) δ 4.57 (d, J=5.81 Hz, 1H), 5.38 (t, J=5.81 Hz, 1H), 7.48 (d, J=8.34 Hz, 2H), 7.78 (d, J=8.34 Hz, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08563723B2 |
| Source dataset | uspto-grants-2013_10 |
| ORD ID | ord-89f0be4b3e8c4ef79190effbddd973ff |
| Source note | uspto-grants-2013_10 |