참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 4-Chloro-3-sulfamoylbenzoic acid | HCID 14568 | — |
| 반응물 | Thionyl Chloride | HCID 24386 | — |
| 반응물 | 2-Ethylbenzofuran | HCID 76582 | — |
| 반응물 | 3-(Aminosulfonyl)-4-chlorobenzoyl chloride | HCID 3017979 | — |
| 반응물 | Aluminum(III) Chloride | HCID 6451240 | — |
| 용매 | Chlorobenzene | HCID 7964 | — |
| 생성물 | 2-Ethyl-3-(4-chloro-3-sulfamoylbenzoyl)-benzo[b]furan | HCID 21316586 | — |
반응 단계
10 mg of powdered 4-chloro-3-sulfamoylbenzoyl chloride (melting point, m.p. 166° C.), prepared from 4-chloro-3-sulfamoylbenzoic acid and thionyl chloride, are introduced into 70 ml of anhydrous chlorobenzene, subsequently 6.32 g of 2-ethylbenzo[b]furan are added, and the reaction mixture is cooled to 0° C. After addition of 11.4 g of anhydrous aluminum chloride, the reaction batch is maintained at a temperature of 5° to 10° C., subsequently stirred for 5 hours at 15° C., and the mixture is then poured into a suspension of 200 g of ice and 10 ml of concentrated hydrochloric acid. After extraction with ethyl acetate and washing with water, the organic phase is stirred for 6 hours with a dilute NaHCO3 solution having a pH of 8.5, dried over magnesium sulfate, and, after evaporation, a light yellow to colorless viscous oil is obtained which crystallizes from petroleum ether. Colorless crystals, m.p. 170°-172° C. (from a small amount of methanol).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04156732 |
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| 출처 데이터셋 | uspto-grants-1979_05 |
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| ORD ID | ord-9b94943a4cff48128432d38db0f93c8b |
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| 출처 메모 | uspto-grants-1979_05 |
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