참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Benzisothiazole | HCID 9225 | — |
| 반응물 | Thionyl Chloride | HCID 24386 | — |
| 반응물 | Chlorine | HCID 24526 | — |
| 반응물 | 2-(Methylthio)benzaldehyde oxime | HCID 786757 | — |
| 용매 | Chlorobenzene | HCID 7964 | — |
| 생성물 | 3-Chloro-1,2-benzisothiazole | HCID 598190 | 96.1% |
반응 단계
In a 300 ml four-necked flask equipped with a stirrer, a thermometer, and a condenser, 100 g of monochlorobenzene was placed in advance, to which 33.4 g (0.2 mol) of 2-(methylthio)benzaldehyde oxime was added under nitrogen atmosphere. 25.2 g (0.21 mol) Of thionyl chloride was added dropwise thereto while stirring at a temperature of from -10° to -15° C. and allowed to react for 1 hour at the same temperature. After the termination of the reaction, 15.6 g (0.22 mol) of chlorine was continuously blown into the reaction mixture containing 1,2-benzisothiazole while stirring at a temperature of from 70° to 80° C. and allowed to react for 1 hour at the same temperature. After the termination of the reaction, the reaction mixture was subjected to distilling off of the solvent and then to distillation under reduced pressure to give 32.6 g of 3-chloro-1,2-benzisothiazole. The yield was 96% to the 2-(methylthio)benzaldehyde oxime.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05856504 |
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| 출처 데이터셋 | uspto-grants-1999_01 |
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| ORD ID | ord-5452ffc334694ae09b9bc88857992547 |
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| 출처 메모 | uspto-grants-1999_01 |
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