Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 4-Nitrobenzenethiol | HCID 15809 | — |
| Reactant | HCID 12832615 | HCID 12832615 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 14275577 | HCID 14275577 | 35.3% |
Reaction Steps
In 30 ml of dichloromethane was dissolved 1.0 g of 4-bromomethyl-1,3-dioxol-2-one, and 0.9 g of 4-nitrobenzenethiol was added. Then, 0.6 g of triethylamine was added, and the mixture was stirred at room temperature for 1 hour. After the reaction, the solvent was evaporated under reduced pressure, and the residue was dissolved in ethyl acetate. The insoluble materials were separated by filtration, and the solvent was evaporated under reduced pressure. The residue was subjected to medium-pressure silica gel column chromatography as in Example 1 [except that the column was eluted with a mixture of chloroform and n-hexane (2/1, v/v)]. The eluate was evaporated under reduced pressure, and the residue was recrystallized from a mixed solvent of chloroform and n-hexane to give 0.5 g of the captioned compound as yellow crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04777267 |
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| Source dataset | uspto-grants-1988_10 |
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| ORD ID | ord-3ee44317c9054ff88ad8d0e7c9714ef5 |
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| Source note | uspto-grants-1988_10 |
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