참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Iodide | HCID 4875 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 1-(2-Chloroethoxy)-4-nitrobenzene | HCID 2764587 | — |
| 반응물 | 3-(1-Piperazinyl)-1,2-benzisothiazole monohydrochloride | HCID 11521711 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 3-{4-[2-(4-Nitro-phenoxy)-ethyl]-piperazin-1-YL}-1,2-benzisothiazole | HCID 21963311 | 114.9% |
반응 단계
Excess dried, −325 mesh potassium carbonate (257 mg, 1.86 mmol) was diluted in 4 mL acetonitrile and 3-piperazin-1-yl-benzoisothiazole hydrochloride (395 mg, 1.55 mmol), catalytic potassium iodide, and 1(2-chloroethoxy)-4-nitrobenzene (250 mg, 1.20 mmol) were added. This mixture was sealed in a Smith microwave vial and heated on the Smith Workstation at 150° C. for 1.5 h. After cooling, the salts were filtered off and washed with acetonitrile and the filtrate was concentrated. The residue was taken up in methylene chloride and washed with water. The organic layer was dried over sodium sulfate, and concentrated to afford 530 mg of a yellow solid. Yield 89%; 92% HPLC purity at 214 nm; mp 115° C.; MS (APCI): 385 [M+H]+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07101886B2 |
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| 출처 데이터셋 | uspto-grants-2006_09 |
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| ORD ID | ord-cee48d3671df4eb092abef4a301d4b0a |
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| 출처 메모 | uspto-grants-2006_09 |
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