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Water → 4-Chloro-2-[[(1-methylethylidene)amino]oxy]benzonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Acetone, oxime | HCID 67180 | — |
| 反応物 | 4-Chloro-2-nitrobenzonitrile | HCID 96924 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-Chloro-2-[[(1-methylethylidene)amino]oxy]benzonitrile | HCID 18796452 | 65.6% |
反応手順
In 75 ml of dry N,N-dimethylformamide was dissolved acetone oxime (1.21 g), followed by potassium tertiary butoxide (1.85 g) and stirred under nitrogen. After 30 minutes, 4-chloro-2-nitro-benzonitrile (2.00 g) was added. After an additional 30 minutes the reaction was poured into water (500 ml) and filtered. The solid was collected and dissolved in DCM (250 ml), dried (MgSO4), and concentrated in vacuo. The resulting solid was recrystallized from ethanol to yield 1.5 g of the product, m.p. 83-84° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05925766 |
| 出典データセット | uspto-grants-1999_07 |
| ORD ID | ord-b0496799b6cd46ba84d9201c0b9b6e22 |
| 出典メモ | uspto-grants-1999_07 |