Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 2-(Tri-n-butylstannyl)thiophene | HCID 2779373 | — |
| Reactant | HCID 86638408 | HCID 86638408 | — |
| Catalyst | Cuprous chloride | HCID 62652 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 86638406 | HCID 86638406 | — |
Reaction Steps
3,4-bis(diethoxyphosphoryl)-2-iodothiophene and different equivalents of copper(I) chloride (commercially available product) indicated in Table 6 were dissolved in DMF, to which 2-tributylstannylthiophene (1.2 equivalents) was added at room temperature. Thereafter, the reaction mixture was heated to 80° C. and stirred for 8.5 to 11 hours. After the reaction, the reaction mixture was cooled down to room temperature, to which a 0.6 M hydrochloric acid aqueous solution was added, 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 (ethyl acetate:methanol=15:1) to obtain the specified substance.
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-f0e7220f03034f70b6d3afe2fd0312c9 |
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| Source note | uspto-grants-2011_10 |
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