참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | Thionyl Chloride | HCID 24386 | — |
| 반응물 | 3-Fluoro-2-hydroxybenzoic acid | HCID 268724 | — |
| 생성물 | Methyl 3-fluoro-2-hydroxybenzoate | HCID 573875 | 94% |
반응 단계
To a solution of 3-fluoro-2-hydroxy-benzoic acid (5.0 g, 32 mmol) in methanol (20 mL) was added thionyl chloride (5.0 g, 42 mmol) dropwise and the reaction mixture was stirred at 40° C. for 3 hours, then heated at 50° C. for 16 hours. The reaction mixture was cooled and concentrated in vacuo and resulting residue was purified by silica gel column chromatography using 0-50% ethyl acetate/hexanes mixtures as eluant to give methyl 3-fluoro-2-hydroxy-benzoate (5.1 g, 94%) as white crystals. ESI-MS m/z calc. 170.0. found 170.9 (M+1)+; Retention time: 1.33 minutes (3 min run).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09181273B2 |
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| 출처 데이터셋 | uspto-grants-2015_11 |
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| ORD ID | ord-7337c420c52a4a328726af9b0ff9f066 |
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| 출처 메모 | uspto-grants-2015_11 |
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