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2-(3,4-Dimethylphenyl)acetonitrile → 2-(3,4-dimethylphenyl)-N'-hydroxyethanimidamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-(3,4-Dimethylphenyl)acetonitrile | HCID 76401 | — |
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 反応物 | Sodium methanolate methanol | HCID 23694274 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2-(3,4-dimethylphenyl)-N'-hydroxyethanimidamide | HCID 5187867 | 93% |
反応手順
3,4-Dimethylphenylacetonitrile (10 g, 0.069 mol) was added to a mixture of hydroxylamine hydrochloride (9.57 g, 0.14 mol), methanol (100 mL) and 25% sodium methoxide/methanol (31.5 mL, 0.14 mol) at room temperature. After stirring for 16 hours at room temperature, the reaction mixture was concentrated in vacuo. The resultant oil was partitioned between methylene chloride and water. The organic phase was separated, washed with water, dried over magnesium sulfate and concentrated in vacuo to yield the desired product (11.4 g, 93%) as a white solid. Recrystallization from toluene afforded an analytical sample m.p. 59°-60° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04895862 |
| 出典データセット | uspto-grants-1990_01 |
| ORD ID | ord-2151eb6996b04815873593e7d1dea55c |
| 出典メモ | uspto-grants-1990_01 |