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Water → 5-Bromo-3-(3-chlorophenyl)-2,1-benzisoxazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 1-Bromo-4-nitrobenzene | HCID 11466 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | m-Chlorophenylacetonitrile | HCID 73722 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 5-Bromo-3-(3-chlorophenyl)-2,1-benzisoxazole | HCID 12016670 | 34.8% |
反応手順
Sodium hydroxide (0.62 mol) was dissolved in methanol (100 ml) and the mixture was cooled till room temperature. 1-bromo-4-nitro-benzene (0.124 mol), followed by 3-chloro-benzeneacetonitrile (0.223 mol) were added dropwise, the temperature raised till 50° C. and the mixture was stirred at room temperature for one night. The mixture was poured into water and ice, the precipitate was filtered off, washed with water and extracted with CH2Cl2 and CH3OH. The organic layer was dried (MgSO4), filtered off and evaporated till dryness. The residue was taken up in Et2O, filtered off and dried, yielding 13.2 g (34.8%) of 5-bromo-3-(3-chlorophenyl)-2,1-benzisoxazole, mp. 163° C. (intermediate 1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07173040B2 |
| 出典データセット | uspto-grants-2007_02 |
| ORD ID | ord-d279aa93bcb64ec0a3f9cb083911bb48 |
| 出典メモ | uspto-grants-2007_02 |