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Hydrogen Peroxide → Dimethyl-[5-(2-methylsulfonylpyrimidin-4-yl)-6-(3-trifluoromethylphenyl)-pyridazin-3-yl]amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrogen Peroxide | HCID 784 | — |
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Dimethyl-[5-(2-methylsulfanylpyrimidin-4-yl)-6-(3-trifluoromethylphenyl)-pyridazin-3-yl]amine | HCID 18176616 | — |
| 触媒 | Sodium tungstate | HCID 26052 | — |
| 生成物 | Dimethyl-[5-(2-methylsulfonylpyrimidin-4-yl)-6-(3-trifluoromethylphenyl)-pyridazin-3-yl]amine | HCID 18176627 | — |
反応手順
Compound 71 (112 mg, 0.286 mmol), sodium tungstate (10 mg, 0.02 mmol), 30% hydrogen peroxide (130 μL, 1.14 mmol), methanol (2.0 mL), and ethyl acetate (20 mL) were combined under Argon and heated to reflux for 3d. The solution was cooled, poured into water and extracted several times with ethyl acetate. The combined organic extracts were dried with anhydrous sodium sulfate. Removal of the solvent in vacuo gave 72 as a solid: 109 mg (0.259 mmol, 91%)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06602872B1 |
| 出典データセット | uspto-grants-2003_08 |
| ORD ID | ord-bd9f0d4d6bbb4dd4b3bc580128c3cb66 |
| 出典メモ | uspto-grants-2003_08 |