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2-Acetoxyisobutyroyl chloride → 1,1-Dimethyl-2-[2-[2-[[4-(methylthio)phenyl]amino]isonicotinoyl]hydrazino]-2-oxoethyl acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Acetoxyisobutyroyl chloride | HCID 123496 | — |
| 反応物 | 2-[[4-(Methylthio)phenyl]amino]isonicotinohydrazide | HCID 68664110 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 生成物 | 1,1-Dimethyl-2-[2-[2-[[4-(methylthio)phenyl]amino]isonicotinoyl]hydrazino]-2-oxoethyl acetate | HCID 68664678 | 83% |
反応手順
To a solution of 2-[[4-(methylthio)phenyl]amino]isonicotinohydrazide (513 mg, 1.87 mmol) in N,N-dimethylacetamide (5 mL) was added dropwise 2-chloro-1,1-dimethyl-2-oxoethyl acetate (0.294 mL, 2.06 mmol) under ice-cooling, and the resulting mixture was stirred at room temperature for 2 hr. The reaction mixture was diluted with ethyl acetate, washed with water and saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was recrystallized from hexane/ethyl acetate to give the title compound (624 mg, yield 83%) as colorless crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08492378B2 |
| 出典データセット | uspto-grants-2013_07 |
| ORD ID | ord-a2830d7d00cf44b386d653326d30cb5e |
| 出典メモ | uspto-grants-2013_07 |