Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | (2,2':5',2''-Terthiophene)-5-carboxaldehyde | HCID 454742 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 54119952 | HCID 54119952 | 70% |
Reaction Steps
3.5 g of 5-formyl-2,2':5',2"-terthiophene was dissolved in 200 ml of anhydrous THF under nitrogen stream. 7.9 ml of ethyl Grignard reagent was dropped in slowly under ice bath temperature and stirred at 0° C. for 1 hour. The reaction mixture was then heated to 70° C. in oil bath for 4 hours. The solution was monitored by thin layer chromatography to determine whether the reaction was completed. 50 ml of water and 300 ml of ethyl acetate were added and the ethyl acetate extract was purified by column chromatography. From the eluate of ethyl acetate/n-hexane (1/9) fraction, yellow solid was obtained and recrystallized to give granulate crystal. The melting point of the product was 89°-90° C. and the yield was about 70%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05602170 |
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| Source dataset | uspto-grants-1997_02 |
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| ORD ID | ord-63825134f1d74ebe839f61f69c36dc82 |
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| Source note | uspto-grants-1997_02 |
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