Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Sulfuryl chloride | HCID 24648 | — |
| Reactant | HCID 178510728 | HCID 178510728 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | 1,1-Dichloroethane | HCID 6365 | — |
| Product | HCID 178510502 | HCID 178510502 | — |
Reaction Steps
2.61 gm (9.61 mmols) of (E)-2-[(amino)-4-fluorophenylmethylene]-benzo[b]thiophen-3(2H)-one were dissolved in 50 ml of dichloromethane, the solution was cooled to -70° C, and then a solution of 1.5 gm (11.1 mmols) of sulfuryl chloride in 5 ml of dichloroethane was added dropwise thereto. After 15 hours, 20 ml of 95% ethanol were added, and the reaction mixture was brought to room temperature by removal of the cooling bath. It was then neutralized with aqueous sodium carbonate, the dichloromethane phase was dried with sodium sulfate, the solvent was evaporated in vacuo, and the residue was recrystallized from glacial acetic acid/ethanol (1:4 v/v).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04536402 |
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| Source dataset | uspto-grants-1985_08 |
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| ORD ID | ord-e25b65f2c08e4d8785798f3cb3bf0e97 |
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| Source note | uspto-grants-1985_08 |
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