참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Phosphorus pentachloride | HCID 24819 | — |
| 반응물 | Sodium 2-carboxy-benzo[b]thiophene-3-sulfonate | HCID 23714405 | — |
| 용매 | Phosphorus oxychloride | HCID 24813 | — |
| 생성물 | HCID 53652618 | HCID 53652618 | — |
반응 단계
44.0 gm (0.157 mol) of the above 2-carboxy-benzo[b]thiophene-3-sulfonic acid mono sodium salt were suspended in 200 cc of phosphorus oxychloride and admixed with 65.4 gm (0.314 mol) of phosphorus-(V)-chloride. To complete the reaction which was exothermic in the beginning accompanied by evolution of hydrogen chloride, the reaction mixture was heated to 100° C. for 2 hours, cooled and the inorganic salts were filtered off. After evaporation in vacuo, the residue was taken up in 300 cc of dry chloroform, the solution was filtered and again evaporated. The oily residue, consisting of 27 gm (58% of theory) of raw 2-chlorocarbonyl-benzo[b]thiophene-3-sulfonic acid chloride, crystallized upon cooling (m.p. 45°-47° C.) and was used without further purification in the next step.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US04259336 |
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| 출처 데이터셋 | uspto-grants-1981_03 |
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| ORD ID | ord-14d096795bba47acbafa6b123602e040 |
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| 출처 메모 | uspto-grants-1981_03 |
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