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Carbon tetrabromide → 5-(2,2-Dibromoethenyl)-2,2'-bithiophene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Carbon tetrabromide | HCID 11205 | — |
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | [2,2'-Bithiophene]-5-carboxaldehyde | HCID 364428 | — |
| 反応物 | 5-Formyl-2,2'-bithiophene dichloromethane | HCID 86750360 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | 5-(2,2-Dibromoethenyl)-2,2'-bithiophene | HCID 13113977 | — |
反応手順
0.55 g of 5-formyl-2,2'-bithiophene was dissolved in 10 ml of dichloromethane. 1.95 g of PPh3 and 1.23 g of CBr4 were dissolved in 40 ml of dichloromethane and mixed with the 5-formyl-2,2'-bithiophene/dichloromethane solution under nitrogen gas atmosphere at 0° C. After the mixture was stirred for 1 hour and 10 ml of n-hexane was added to precipitate the triphenyl-phosphine oxide. And the reaction solution was filtered. Further, 100 ml of n-hexane was then added into the solution and the yellowish solid was obtained. The solid was further purified by column chromatography and crystallized with ethanol. The crystal product was thus obtained and the melting point thereof was 112°-113° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05753692 |
| 出典データセット | uspto-grants-1998_05 |
| ORD ID | ord-aaf308b26b4341b194b4671fb63e979e |
| 出典メモ | uspto-grants-1998_05 |