関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) | HCID 466102 | — |
| 反応物 | Andrographolide | HCID 5318517 | — |
| 反応物 | Dimethylsulfoxide toluene | HCID 22340214 | — |
| 溶媒 | 2,2-Dimethoxypropane | HCID 6495 | — |
| 生成物 | HCID 16122395 | HCID 16122395 | 2,788.6% |
反応手順
Andrographolide (150 mg, 0.43 mmol) was dissolved in a mixture solution of 2,2-dimethoxypropane (0.2 mL), pyridinium p-toluene-sulfonate (3 mg) and toluene/DMSO (3 mL/0.4 mL), stirred at 80° C. for 1 hour, and cooled to room temperature at the end. The reaction was terminated by using triethylamine (0.1 mL), the reaction mixture was diluted with toluene (20 mL), washed with water (3×5 mL), the organic layer was dried using anhydrous Na2SO4 and concentrated, and the obtained white solid was washed with ethyl ether and filtrated to obtain the compound 1 (130 mg, 78%) (Srinivas et al., Bioorg. Med. Chem. Lett. 2004, 14, 4711-4717).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08367720B2 |
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| 出典データセット | uspto-grants-2013_02 |
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| ORD ID | ord-8b4b80bd476f494ea0edaec42d30e49b |
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| 出典メモ | uspto-grants-2013_02 |
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