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Ethylenediamine → N-(2-Aminoethyl)-4-chlorobenzamide hydrochloride

HRID 2255109
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HRID 2255109 반응식
[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6](Cl)=[O:7])=[CH:4][CH:3]=1.[CH2:11]([NH2:14])[CH2:12][NH2:13]>CCOCC>[ClH:1].[NH2:13][CH2:12][CH2:11][NH:14][C:6](=[O:7])[C:5]1[CH:9]=[CH:10][C:2]([Cl:1])=[CH:3][CH:4]=1
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참가 물질

4

반응물 2

HCID 3301EthylenediamineHCID 85014-Chlorobenzoyl chloride

생성물 1

HCID 5702251N-(2-Aminoethyl)-4-chlorobenzamide hydrochloride수율 30.6%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

A solution of 6.2 ml (0.05 mol) of 4-chlorobenzoyl chloride in 150 ml of ether is added dropwise at -10° over a period of 0.5 hour to a solution of 10 ml (0.15 mol) of ethylenediamine in 150 ml of ether. The mixture is left to warm to room temperature, filtered and the white residue is rinsed twice with ether. After concentrating the ether solution, the residue is acidified with dilute hydrochloric acid and extracted several times with ethyl acetate in order to remove the neutral constituents. The aqueous phase is made alkaline with sodium hydroxide solution and extracted several times with chloroform. After evaporating the chloroform, converting the residue into the hydrochloride and recrystallization from ethanol/ether, there are obtained 1.8 g of N-(2-aminoethyl)-4-chlorobenzamide hydrochloride which is identical with the product obtained in Example 1.

후처리

  1. waitThe mixture is left
  2. filtrationfiltered
  3. washthe white residue is rinsed twice with ether
  4. concentrationAfter concentrating the ether solution
  5. extractionextracted several times with ethyl acetate in order
  6. customto remove the neutral constituents
  7. extractionextracted several times with chloroform
  8. customAfter evaporating the chloroform
  9. custominto the hydrochloride and recrystallization from ethanol/ether, there

출처 및 근거

ORD 기록
ord-87730b0b2e494be4901dc4d3092e09e7
출처 데이터셋
uspto-grants-1993_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05238962

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