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 | Aluminum(III) Chloride | HCID 6451240 | — |
| 反応物 | 2,6-Dichloro-5'-nitro-4'-methoxy-2'-methyl-benzophenone | HCID 54492291 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2,6-Dichloro-4'-hydroxy-5'-nitro-2'-methyl-benzophenone | HCID 53907643 | — |
反応手順
Aluminumchloride (1.5 g; 11 mmol) is added to a solution of 2,6-dichloro-5'-nitro-4'-methoxy-2'-methyl-benzophenone (1.8 g; 5.3 mmol) in methylenechloride (6 ml). The mixture is stirred for 30 minutes at 20° C. and for 1 hour at 45° C., 5 ml conc. hydrochloric acid/ice are added. After shaking with 20 ml of methylenechloride the organic layer is treated with 2N hydrochloric acid and with water. After drying the solvent is evaporated, the residue purified by chromatography (flash column filled with 30 g of silicagel, elution with toluene). The residue from the main fraction is treated with diisopropylether to give yellow crystalls; (1.2 g; 73% y); mp. 170° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05922919 |
|---|
| 出典データセット | uspto-grants-1999_07 |
|---|
| ORD ID | ord-c2b2af1b757e4af992df4ba7376ddb8f |
|---|
| 出典メモ | uspto-grants-1999_07 |
|---|