참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Lawesson's reagent | HCID 87949 | — |
| 반응물 | HCID 178448490 | HCID 178448490 | — |
| 용매 | Toluene | HCID 1140 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | HCID 178448493 | HCID 178448493 | — |
반응 단계
To a solution of Example 6B (1.4 g, 3.7 mmol) in toluene (50 mL) was added Lawesson's reagent (1.6 g, 4 mmol) and the mixture was refluxed at 80° C. for 30 minutes. After cooling to room temperature, the mixture was diluted with EtOAc, washed with 10% solution of bicarbonate, brine and dried with anhydrous MgSO4, filtered and concentrated under reduced pressure. Purification by column chromatography (2:1 Hexane-EtOAc) provided the title compound. 1H NMR (300 MHz, DMSO-d6) δ: 0.89 (t, J=7 Hz, 3H), 1.25 (sextet, J=7 Hz, 2H), 1.36 (s, 9H), 1.76 (m, 2H), 3.74 (s, 3H), 4.25 (t, J=7 Hz, 2H), 7.06 (d, J=9 Hz, 1H), 7.35 (m, 2H), 7.45 (s, 1H); MS (ESI+) m/z 397 (M+H)+. Anal. calcd for C19H25ClN2OS2: C, 57.48; H, 6.35; N, 7.06. Found: C, 57.26; H, 6.17; N, 6.79.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07875640B2 |
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| 출처 데이터셋 | uspto-grants-2011_01 |
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| ORD ID | ord-0ad203745b294f32b6160bb0f93da04a |
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| 출처 메모 | uspto-grants-2011_01 |
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