참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hexane | HCID 8058 | — |
| 반응물 | Dihexylamine | HCID 8920 | — |
| 반응물 | 2-Methyl-1,3-benzothiazole-6-sulfonyl chloride | HCID 3583019 | — |
| 용매 | Chloroform | HCID 6212 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | N,N-dihexyl-2-methylbenzo[d]thiazole-6-sulfonamide | HCID 57796621 | 97% |
반응 단계
A solution of compound Compound 2 (5.0 g, 20.2 mmol) from step (b) of Example 1 dissolved in chloroform (30 ml) was added drop wise to a solution of dihexylamine (4.5 g, 24.2 mmol) in chloroform (20 ml). The combined mixture was stirred at room temperature for 2 hours. The reaction mixture was then washed with water (2×, 50 ml) and brine (1×, 50 ml). The organic layer was then dried with sodium sulfate and evaporated. The residue thus obtained was suspended in ca. 5 ml hot ethyl acetate and this solution was then slowly added to 40 ml hexane. The white solid that precipitated was filtered and the filtrate evaporated to dryness to provide 7.76 g (97%) of Compound 20 as a syrupy liquid, Rf=0.43 (30% ethyl acetate in hexane). The structure of this compound is given below:
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08759526B2 |
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| 출처 데이터셋 | uspto-grants-2014_06 |
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| ORD ID | ord-03c164f795cf41fab7f5467591e93c57 |
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| 출처 메모 | uspto-grants-2014_06 |
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