Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Sodium sulfide nonahydrate | HCID 73972 | — |
| Reactant | 3-Bromo-4-thiocyanatophenol | HCID 71362151 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 69514021 | HCID 69514021 | 92.2% |
Reaction Steps
To a hot (85° C.) solution of 3-bromo-4-thiocyanato-phenol (315 mg, 1.37 mmol) in absolute ethanol (10 mL) under nitrogen, sodium sulfide nonahydrate (403 mg, 2.05 mmol) was added. The resulting mixture was stirred at 85° C. for 20 min. More sodium sulfide nonahydrate (230 mg) was added and heating was continued for 15 min. The mixture was cooled down, made acidic with 5N acetic acid (10 mL) and extracted with methylene chloride (×1). The organic layer was washed once with water, dried and concentrated in vacuo to give the title compound as a yellow solid (259 mg, 92%) which was quickly submitted to the next reaction without further treatment. EIMS M−1: 203.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07148236B2 |
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| Source dataset | uspto-grants-2006_12 |
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| ORD ID | ord-0c171be188214721b2b5031767d87b28 |
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| Source note | uspto-grants-2006_12 |
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