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Methylamine → 4-(Methylaminomethyl)benzonitrile

HRID 1856719
ノート
印刷プレビュー

反応式

HRID 1856719 の反応式
[CH:1]1[C:6]([CH2:7]Br)=[CH:5][CH:4]=[C:3]([C:9]#[N:10])[CH:2]=1.[CH3:11][NH2:12]>C(#N)C>[CH3:11][NH:12][CH2:7][C:6]1[CH:5]=[CH:4][C:3]([C:9]#[N:10])=[CH:2][CH:1]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6329MethylamineHCID 869964-(Bromomethyl)benzonitrile

生成物 1

HCID 106068834-(Methylaminomethyl)benzonitrile収率 38.6%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

実験手順

A solution of a-bromo-p-tolunitrile (4.90 g, 25 mmol) in acetonitrile (50 mL) was added dropwise to a stirring solution of 40% aqueous methylamine (21.5 mL, 250 mmol) in acetonitrile (50 mL) at 0° C. The reaction mixture was stirred 0.5 h, then concentrated in vacua. Water was added to the residue and extracted 2× with dichloromethane. The combined organic layers were dried over sodium sulfate, filtered, and concentrated in vacua to give 1.41 g of 4-(methylaminomethyl)benzonitrile as a yellow oil containing ~30% of N,N-bis(4-benzonitrile)methyl-amine. The aqueous was adjusted to pH>8 and extracted 2× with 9:1 dichloromethane:methanol. The combined extracts were dried over sodium sulfate, filtered, and concentrated in vacua to give 1.13 g of pure 4-(methylamino)benzonitrile as a colorless oil.

後処理

  1. concentrationconcentrated in vacua
  2. additionWater was added to the residue
  3. extractionextracted 2× with dichloromethane
  4. dry with materialThe combined organic layers were dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacua

出典と根拠

ORDレコード
ord-1eac827d4166434b909cde60cb695418
出典データセット
uspto-grants-2000_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06143760

反応ノート

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