HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-(Tri-n-butylstannyl)thiophene → 3-Diethoxyphosphoryl-[2,2']-bithiophene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-(Tri-n-butylstannyl)thiophene | HCID 2779373 | — |
| Reactant | 2-Iodo-3-diethoxyphosphorylthiophene | HCID 59155836 | — |
| Catalyst | Cuprous chloride | HCID 62652 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 3-Diethoxyphosphoryl-[2,2']-bithiophene | HCID 59155828 | — |
Reaction Steps
Copper(I) chloride (2.5 equivalents) was charged into a reaction container, to which 2-thienyltributyl tin (2.5 equivalents) and 2-iodo-3-diethoxyphosphorylthiophene were added under nitrogen atmosphere while being dissolved in tetrahydrofuran, followed by heating under reflux for 20 hours. After completion of the reaction, the reaction solution was filtered through celite and the resulting residue was washed with ethyl acetate. The filtrate was washed three times with a 1N hydrochloric acid aqueous solution and a 10% saline solution and dried over anhydrous sodium sulfate. The solvent was distilled off, and the resulting crude product was purified with a silica gel column (hexane:ethyl acetate=1:3) to obtain a colorless liquid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08030438B2 |
| Source dataset | uspto-grants-2011_10 |
| ORD ID | ord-2055e280654845ffbbfc71d2e378ae04 |
| Source note | uspto-grants-2011_10 |