HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 57663184, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 43501950 | HCID 43501950 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 57663184 | HCID 57663184 | 28.1% |
Reaction Steps
Sodium hydride (60% dispersion in mineral oil) (260 mg, 6.49 mmol) was added to a solution of 2,4-difluoro-N-(2-hydroxyethyl)benzenesulfonamide (0.7 g, 2.95 mmol) in DMF (100 mL) and the mixture stirred at RT for 48 hours. The solvent was removed in vacuo, iced water (200 mL) added and the mixture extracted into ethyl acetate. The combined organic extracts were washed with brine (40 mL), dried (MgSO4), filtered and reduced in vacuo to give a white solid which was chromatographed on silica, eluting with 20-70% ethyl acetate in isohexane, to give the desired compound as a white solid (0.18 g). 1H NMR δ (CDCl3): 3.65-3.70 (m, 2H), 4.25-4.27 (m, 2H), 4.69 (t, 1H), 6.86-6.94 (m, 2H), 7.82-7.86 (m, 1H); m/z 216 (M−H)−
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07943607B2 |
| Source dataset | uspto-grants-2011_05 |
| ORD ID | ord-3f1f031157d941728efe102e78b831f7 |
| Source note | uspto-grants-2011_05 |