関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzene | HCID 241 | — |
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 反応物 | 5,7-Di-tert-butyl-3-hydroxy-2-benzofuranone | HCID 6850821 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5,7-Bis(1,1-dimethylethyl)-3-phenyl-(3H)-benzofuran-2-one | HCID 6455356 | 64% |
反応手順
73.3 g (0.55 mol) of ground aluminium trichloride are added over 25 minutes to a solution of 131.2 g (0.50 mol) of 5,7-di-tert-butyl-3-hydroxy-3H-benzofuran-2-one (compound (201), Table 2, Example 1a) in 250 ml (2.82 mol) of benzene and the reaction mixture is heated for 1.5 hours to reflux temperature and then refluxed for 1.5 hours. The reaction mixture is cooled to room temperature and then, cautiously with cooling, 200 ml of water are added, followed by the addition of concentrated hydrochloric acid until a homogeneous two-phase mixture forms. The organic phase is separated, washed with water, dried over sodium sulfate and concentrated on a vacuum rotary evaporator. Crystallisation of the residue from ethanol yields 97.8 g (64%) of 5,7-di-tert-butyl-3-phenyl-3H-benzofuran-2-one, m.p. 116°-119° C. (compound (108), Table 1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05607624 |
|---|
| 出典データセット | uspto-grants-1997_03 |
|---|
| ORD ID | ord-bc04b285dcab43c4ba34a66dff0845d8 |
|---|
| 出典メモ | uspto-grants-1997_03 |
|---|