3,5-Dichloroaniline → HCID 19978192, 화합물

HRID 1449504노트

반응식

HRID 1449504 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:6]=[C:7]([Cl:9])[CH:8]=1)[NH2:5].Br[CH2:11][CH2:12][C:13]([O:15][CH2:16][CH3:17])=[O:14]>CN(C)C=O>[CH2:16]([O:15][C:13]([CH2:12][CH2:11][NH:5][C:4]1[CH:3]=[C:2]([Cl:1])[CH:8]=[C:7]([Cl:9])[CH:6]=1)=[O:14])[CH3:17]

참가 물질

4

반응물 2

HCID 122813,5-DichloroanilineHCID 68320Ethyl 3-bromopropionate

생성물 1

HCID 19978192HCID 19978192, 화합물수율 49.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

In 20 ml of dimethylformamide was dissolved 5.0 g of 3,5-dichloroaniline. To the solution was added 6.16 g of ethyl 3-bromopropionate, followed by heating under reflux for 6 hours. The reaction mixture was concentrated and the concentrate was extracted with ethyl acetate. The extract was washed with saturated sodium hydrogencarbonate aqueous solution and saturated sodium chloride aqueous solution and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure. The residue was subjected-to silica gel column chromatography (eluent: chloroform:hexane=1:1) to yield 3.98 g of the titled compound as a white crystal.

후처리

  1. temperatureby heating
  2. temperatureunder reflux for 6 hours
  3. concentrationThe reaction mixture was concentrated
  4. extractionthe concentrate was extracted with ethyl acetate
  5. washThe extract was washed with saturated sodium hydrogencarbonate aqueous solution and saturated sodium chloride aqueous solution
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customThe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-f34c84f955864d789d016137a0f23747
출처 데이터셋
uspto-grants-1997_02
특허 번호
US05599813

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