HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 86703887, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 4-Bromo-3,5-dimethylphenol | HCID 81970 | — |
| Reactant | HCID 57794291 | HCID 57794291 | — |
| Product | HCID 86703887 | HCID 86703887 | — |
Reaction Steps
4-Bromo-3,5-dimethylphenol (1.25 g, 6.17 mmol) and sodium hydride (60% on mineral oil, 160 mg, 3.95 mmol) are suspended in dry N,N-dimethylacetate (25 mL) and stirred for 30 minutes at room temperature. Methanesulfonic acid 2-(1,1-dioxo-isothiazolidin-2-yl)-ethyl ester (Patent EP1479684 A1, 600 mg, 2.47 mmol;) is added and the mixture stirred at 80° C. for 5 hours. The mixture is concentrated under vacuum, diluted with water and extracted with ethyl acetate. The organic phase is dried and the solvent removed. The residue is purified by flash chromatography (0-50% ethyl acetate in cyclohexane) to give the title compound. (Yield: 350 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08633182B2 |
| Source dataset | uspto-grants-2014_01 |
| ORD ID | ord-5bfcdb716c8040d29c9fbf09b13a14b9 |
| Source note | uspto-grants-2014_01 |