Diethylamine → (E)-4-(4-Chlorophenyl)-N,N-diethyl-2-buten-1-amine

HRID 464025ノート

反応式

HRID 464025 の反応式
[CH2:1]([NH:3][CH2:4][CH3:5])[CH3:2].[Cl:6][C:7]1[CH:12]=[CH:11][C:10]([CH2:13]/[CH:14]=[CH:15]/[CH2:16]Cl)=[CH:9][CH:8]=1.ClC1C=CC(CC(Cl)C=C)=CC=1>Cl>[Cl:6][C:7]1[CH:12]=[CH:11][C:10]([CH2:13]/[CH:14]=[CH:15]/[CH2:16][N:3]([CH2:4][CH3:5])[CH2:1][CH3:2])=[CH:9][CH:8]=1

参加物

5

反応物 3

HCID 8021DiethylamineHCID 12616294(E)-1-chloro-4-(4-chloro-2-butenyl)benzeneHCID 136602341-Chloro-4-(2-chloro-3-butenyl)benzene

生成物 1

HCID 20263609(E)-4-(4-Chlorophenyl)-N,N-diethyl-2-buten-1-amine

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

Add 30 ml diethylamine to 10.0 g (0.05 mole) of a 7:3 mixture of (E)-1-chloro-4-(4-chloro-2-butenyl)benzene and 1-chloro-4-(2-chloro-3-butenyl)benzene and stir at room temperature overnight. Dissolve reaction mixture in 100 ml 1N HCl and wash with 50 ml ethyl acetate. Extract ethyl acetate layer with 50 ml 1N HCl. Combine aqueous layers and add cold 4N NaOH until solution has pH=9. Extract aqueous phase with 5×60 ml Et2O. Dry ethereal extracts over Na2SO4 and then filter. Evaporate solvent to provide the title compound.

後処理

  1. dissolutionDissolve
  2. washwash with 50 ml ethyl acetate
  3. additionCombine aqueous layers and add cold 4N NaOH until solution
  4. dry with materialDry ethereal extracts over Na2SO4
  5. filtrationfilter

出典と根拠

ORDレコード
ord-24b85db2c74244f8ac520934d23f4f98
出典データセット
uspto-grants-1985_10
特許番号
US04545995

反応ノート

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