참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Phosphorus oxychloride | HCID 24813 | — |
| 반응물 | Sulfolane | HCID 31347 | — |
| 반응물 | Benzenesulfonic acid, 2-chloro-5-nitro-, sodium salt (1:1) | HCID 70350 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 2-Chloro-5-nitrobenzenesulfonyl chloride | HCID 20630 | — |
반응 단계
To a mixture of 104 g of commercially available sodium 2-chloro-5-nitrobenzenesulfonate, 200 ml of acetonitrile and 200 ml of sulfolane stirred at 25° C., was added 153 ml of phosphorus oxychloride over a period of 30 minutes. The temperature was not allowed to exceed 40° C. After completion of the addition, the reaction mixture was heated to 70° C. for 1.5 hours. On cooling to 0° C., the reaction mixture was poured over ice. The resulting solid product was washed with cold water, filtered and air-dried to give 77.6 g of the title compound with a melting point of 87°-89° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05486610 |
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| 출처 데이터셋 | uspto-grants-1996_01 |
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| ORD ID | ord-d54bc8b308fa4f97afa0bc5e95f44a26 |
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| 출처 메모 | uspto-grants-1996_01 |
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