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

HRID 464025노트

반응식

HRID 464025 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-24b85db2c74244f8ac520934d23f4f98
출처 데이터셋
uspto-grants-1985_10
특허 번호
US04545995

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