Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 4-Methoxybenzenethiol | HCID 12765 | — |
| Reactant | 4-(Chloromethyl)-5-methyl-1,3-dioxol-2-one | HCID 9855518 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 14275572 | HCID 14275572 | 67.7% |
Reaction Steps
In 40 ml of dichloromethane was dissolved 2.0 g of 4-chloromethyl-5-methyl-1,3-dioxol-2-one, and 1.9 g of 4-methoxybenzenethiol was added. Then, 1.4 g of triethylamine was added, and the mixture was stirred at room temperature for 30 minutes. After the reaction, the solvent was evaporated under reduced pressure. 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. The eluate was evaporated under reduced pressure, and the residue was recrystallized from a mixed solvent of ethyl acetate and n-hexane to give 2.3 g of the captioned compound as pale 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-f29697fd1f0541d893de3d9c0750e301 |
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| Source note | uspto-grants-1988_10 |
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