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Hydrochloric Acid → HCID 15267964、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | (1,1'-Biphenyl)-2,2'-dicarboxylic acid, 4,4'-dinitro- | HCID 97509 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 15267964 | HCID 15267964 | — |
反応手順
80 g (241 mmol) 4,4′-Dinitro-1,1′-biphenyl-2,2′-dicarboxylic acid are dissolved in 225 ml THF and added dropwise in the course of 1 hour to 1.4 L (1440 mmol) of a borane-tetrahydrofuran complex 1.0 M solution in THF. After 19 hours at 25° C., 500 ml of water are carefully added. After 1 hour, the solution is acidified to pH=1-2 with 30 ml of 1N HCl solution and allowed to stirred for 30 min. The reaction mixture is then partitioned between ethyl acetate and water. The organic phase is washed repeatedly with water, dried over sodium sulfate, filtered and concentrated by rotary evaporation. The residue, 48 g (66%) of 2,2′-bis(hydroxymethyl)-4,4′-dinitro-1,1′-biphenyl as white powder is used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09334366B2 |
| 出典データセット | uspto-grants-2016_05 |
| ORD ID | ord-13e301d3f8b6427b8583f3952c60cbcd |
| 出典メモ | uspto-grants-2016_05 |