2-(3,4-Dimethylphenyl)acetonitrile → 2-(3,4-dimethylphenyl)-N'-hydroxyethanimidamide

HRID 330250

反応式

HRID 330250 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([CH2:9][C:10]#[N:11])[CH:5]=[CH:6][C:7]=1[CH3:8].Cl.[NH2:13][OH:14].C[O-].[Na+].CO>CO>[OH:14][N:13]=[C:10]([NH2:11])[CH2:9][C:4]1[CH:5]=[CH:6][C:7]([CH3:8])=[C:2]([CH3:1])[CH:3]=1

参加物

5

反応物 3

HCID 764012-(3,4-Dimethylphenyl)acetonitrileHCID 443297Hydroxyamine hydrochlorideHCID 23694274Sodium methanolate methanol

生成物 1

HCID 51878672-(3,4-dimethylphenyl)-N'-hydroxyethanimidamide収率 93%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  1. concentrationthe reaction mixture was concentrated in vacuo
  2. customThe resultant oil was partitioned between methylene chloride and water
  3. customThe organic phase was separated
  4. washwashed with water
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-2151eb6996b04815873593e7d1dea55c
出典データセット
uspto-grants-1990_01
特許番号
US04895862

関連ノート

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