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Dichlorodiphenylmethane → 5-Bromo-6-fluoro-2,2-diphenyl-2H-1,3-benzodioxole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dichlorodiphenylmethane | HCID 16327 | — |
| 反応物 | 4-Bromo-5-fluorobenzene-1,2-diol | HCID 21865378 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 5-Bromo-6-fluoro-2,2-diphenyl-2H-1,3-benzodioxole | HCID 21865386 | — |
反応手順
A mixture of 4-bromo-5-fluoro-benzene-1,2-diol (12 g, 58.0 mmol) and diphenyldichloromethane (1.2 eq., 16.50 g) was stirred at room temperature until gaseous evolution ceased. The mixture was heated with stirring at 180° C. for 20 min. The reaction mixture was allowed to cool to room temperature, diluted with methanol (50 ml) and vigorously stirred. The precipitated product was collected by filtration and dissolved in toluene (50 ml). Methanol (100 ml) was added and the mixture stirred 30 min at room temperature. The precipitated product was collected by filtration (yield 10.3 g, 48%), a further batch (6.4 g, 30%) was recovered from the mother liquors.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07144890B2 |
| 出典データセット | uspto-grants-2006_12 |
| ORD ID | ord-22babda1248e44f190352129f071a9c2 |
| 出典メモ | uspto-grants-2006_12 |