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Sulfuric Acid → alpha-(3,4-Dimethoxy-5-nitrophenyl)-2-thiophenemethanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Thiophene | HCID 8030 | — |
| 反応物 | 3,4-Dimethoxy-5-nitrobenzaldehyde | HCID 10867565 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | alpha-(3,4-Dimethoxy-5-nitrophenyl)-2-thiophenemethanol | HCID 21458951 | — |
反応手順
18.8 ml of n-butyllithium solution (1.6M in hexane) are added dropwise at -50° within 10 minutes to 4.03 g of thiophene dissolved in 40 ml of tetrahydrofuran. After stirring at -50° for 30 minutes 6.3 g of 3,4-dimethoxy-5-nitrobenzaldehyde dissolved in 100 ml of tetrahydrofuran are added dropwise within 30 minutes. The reaction mixture is stirred at -50° for 1 hour at 0° for 30 minutes and poured into 100 ml of 2N sulphuric acid. The mixture is extracted three times with 100 ml of ether each time: the combined ether phases are washed with sodium chloride solution, dried over sodium sulfate, filtered and evaporated. There is obtained α-(3,4-dimethoxy-5-nitrophenyl)-2-thiophenemethanol of m.p. 79°-81° (from methylene chloride/hexane).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05389653 |
| 出典データセット | uspto-grants-1995_02 |
| ORD ID | ord-598d92f0fdcb4f39b6836b0fec46cdf7 |
| 出典メモ | uspto-grants-1995_02 |