Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | N-Iodosuccinimide | HCID 120273 | — |
| Reactant | 3-(Diethoxyphosphoryl)thiophene | HCID 15363303 | — |
| Reactant | Sodium phosphate (Na3(PO4)2) | HCID 86630341 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 59155826 | HCID 59155826 | 73% |
Reaction Steps
In 5 ml of a mixed solvent of chloroform:acetic acid=1:1, 0.1101 g (0.5 mmols) of 3-(diethoxyphosphoryl)thiophene was dissolved, to which 0.2362 g (1.05 mmols) of commercially available N-iodosuccinimide was added at room temperature. Thereafter, the reaction mixture was stirred at room temperature for 4 days. After the reaction, a disodium hydrogen phosphate/sodium dihydrogen phosphate buffer solution, adjusted to pH=7, was added, followed by extraction with chloroform. The organic phase was washed with a 0.2N sodium hydroxide aqueous solution and dried over anhydrous sodium sulfate. The solvent was removed, and the resulting crude product was purified with a PTLC plate (developed with ethyl acetate:hexane 1:1) to obtain the specified substance in the form of a yellow oil at a yield of 0.1263 g (yield: 73%). The thus obtained substance was used as it is for reaction in Example 12(9).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08030438B2 |
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| Source dataset | uspto-grants-2011_10 |
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| ORD ID | ord-e62db8f22eda466ab3e1fcec2b31b9bd |
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| Source note | uspto-grants-2011_10 |
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