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Hydrochloric Acid → 2-(4-Chloro-3-sulfamoylbenzoyl)-benzo[b]furan
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Salicylaldehyde | HCID 6998 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Bromo-4'-chloro-3'-sulfamoylacetophenone | HCID 12952390 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-(4-Chloro-3-sulfamoylbenzoyl)-benzo[b]furan | HCID 21316593 | — |
反応手順
4 g 2-Bromo-4'-chloro-3'-sulfamoylacetophenone and 1.63 g salicylaldehyde are maintained for 2 hours with agitation and with exclusion of moisture at a temperature of 80° C. in 50 ml anhydrous dimethyl formamide, in the presence of 2.9 g potassium carbonate ground under anhydrous conditions. After cooling, the batch is poured into a mixture of icewater and excess hydrochloric acid, extracted with ethyl acetate and dried over sodium sulfate. After having distilled off the solvent, crystallization is carried out from di-isopropyl ether and isopropanol. M.p. 152°-156° C. Recrystallization from glacial acetic acid after clarification with active charcoal gives colorless crystals having a melting point of 167°-170° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04156732 |
| 出典データセット | uspto-grants-1979_05 |
| ORD ID | ord-be87ce7bc2cb4532b71c9d0edfccb620 |
| 出典メモ | uspto-grants-1979_05 |