Ammonia → HCID 66911322、化合物

HRID 128176

反応式

HRID 128176 の反応式
N.[Na].[C:3](#[N:5])[CH3:4].[Cl:6][C:7]1[CH:14]=[C:13]([Cl:15])[CH:12]=[CH:11][C:8]=1[C:9]#[N:10]>O1CCCC1.C(OCC)C>[NH2:10][C:9]([C:8]1[CH:11]=[CH:12][C:13]([Cl:15])=[CH:14][C:7]=1[Cl:6])=[CH:4][C:3]#[N:5]

参加物

7

反応物 4

HCID 222Ammonia2 回HCID 6342AcetonitrileHCID 810502,4-DichlorobenzonitrileHCID 5360545Sodium2 回

生成物 1

HCID 66911322HCID 66911322、化合物

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A 150 ml. portion of ammonia is condensed in a reaction flask and a small piece of sodium is added. The blue color is discharged by the addition of ferric chloride and 3.22 g. of sodium are added. After the color is discharged, 5.75 ml. of acetonitrile in 10 ml. of diethyl ether are added. The reaction is cooled in a dry ice-acetone bath and 16.6 g. of 2,4-dichlorobenzonitrile in 25 ml. of tetrahydrofuran are added dropwise. The ammonia is allowed to evaporate, the solvent is blown off with nitrogen and water is added. The mixture is extracted with methylene chloride. The organic extracts are dried over sodium sulfate and filtered through Magnesol®. The filtrate is evaporated with the addition of hexanes giving β-amino-2,4-dichlorocinnamonitrile as a white crystalline solid.

後処理

  1. customcondensed in a reaction flask
  2. temperatureThe reaction is cooled in a dry ice-acetone bath
  3. customto evaporate
  4. additionis added
  5. extractionThe mixture is extracted with methylene chloride
  6. dry with materialThe organic extracts are dried over sodium sulfate
  7. filtrationfiltered through Magnesol®
  8. customThe filtrate is evaporated with the addition of hexanes

出典と根拠

ORDレコード
ord-dd048b94224743e08eb1b84638c779d4
出典データセット
uspto-grants-1981_03
特許番号
US04259256

関連ノート

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