참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Sodium sulfide nonahydrate | HCID 73972 | — |
| 반응물 | N-(2-chloro-5-nitrophenyl)-4-methylbenzamide | HCID 3330399 | — |
| 반응물 | Sulfur | HCID 5362487 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 5-Nitro-2-p-tolylbenzo[d]thiazole | HCID 22153305 | 43% |
반응 단계
Sodium sulfide nonahydrate (875 mg, 3.78 mmol) and sulfur (120 mg, 3.78 mmol) were heated until molten. The water was driven off with nitrogen to give a solid. The obtained solid was added in portions to N-(2-chloro-5-nitrophenyl)-4-methylbenzamide (1 g, 3.44 mmol) in ethanol (20 mL) at 85° C. The solution was stirred at 85° C. for 3 h. After cooling, 2M aqueous HCl was added, and the solution was extracted three times with ethyl acetate. The combined organic layers were dried over anhydrous MgSO4 and evaporated. The resulting solid was purified by column chromatography eluting with ethyl acetate/hexanes 10:90 v/v to afford 400 mg (43%) of the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08501713B2 |
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| 출처 데이터셋 | uspto-grants-2013_08 |
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| ORD ID | ord-92cee1e69dff4d2c816103ea4cdda82f |
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| 출처 메모 | uspto-grants-2013_08 |
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