참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Riluzole | HCID 5070 | — |
| 반응물 | Isoamyl Nitrite | HCID 8053 | — |
| 촉매 | Cupric Chloride | HCID 24014 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 2-Chloro-6-(trifluoromethoxy)-1,3-benzothiazole | HCID 10037924 | — |
반응 단계
To a solution containing dry copper (II) chloride (3.44 g, 25.62 mmol) and tri(ethylene glycol)dimethyl ether (10 g) in acetonitrile (150 mL) was added isoamyl nitrite (4.5 mL, 32.02 mmol). The reaction mixture was stirred at rt under argon for 30 minutes. To this suspension was added dropwise, a solution containing 6-trifluoromethoxy-1,3-benzothiazol-2-ylamine (5 g, 21.35 mmol) and tri(ethylene glycol)dimethyl ether (10 g). The reaction mixture was stirred at rt for 10 minutes, and then heated at 50° C. for 3 h. The mixture was cooled to rt, poured cautiously into aqueous 6 N HCl, and extracted with ethyl acetate. The organic layer was washed with 1N aqueous HCl and brine, and concentrated under reduced pressure to give the desired compound in near-quantitative yield, which was used without further purification in the next step.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07423156B2 |
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| 출처 데이터셋 | uspto-grants-2008_09 |
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| ORD ID | ord-4c10f766ee7b4068b4ed47ec95da60b6 |
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| 출처 메모 | uspto-grants-2008_09 |
|---|