Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 59155822 | HCID 59155822 | — |
| Reactant | HCID 59155872 | HCID 59155872 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Cuprous chloride | HCID 62652 | — |
| Product | HCID 86638415 | HCID 86638415 | 55% |
Reaction Steps
At room temperature, 0.8045 g (2.00 mmols) of 3-(dibutoxyphosphoryl)-2-iodothiophene and 1.1308 g (2.00 mmols) of 2-(tributylstannyl)-3-(dibutoxyphosphoryl)thiophene were dissolved in DMF, to which 0.2376 g (2.40 mmols) of commercially available copper(I) chloride was added at room temperature. Thereafter, the reaction mixture was heated to 80° C. and stirred for 10 hours. After the reaction, the reaction mixture was cooled down to room temperature, to which a 10% hydrochloric acid aqueous solution, followed by extraction of the resulting product with ethyl acetate. The organic phase was washed with a saturated saline solution and dried over anhydrous sodium sulfate. The solvent was removed by distilling off under reduced pressure, and the resulting crude product was purified with a silica gel column (gradiated from ethyl acetate:hexane=1:1 with acetone) to obtain the specified substance in the form of white crystals at a yield of 1.6012 g (yield: 55%).
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-b5c8c4e7e91b4011b17f3ca37120b304 |
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| Source note | uspto-grants-2011_10 |
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