3,5-Dichloroaniline → HCID 19978192、化合物

HRID 1449504ノート

反応式

HRID 1449504 の反応式
[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]

参加物

4

反応物 2

HCID 122813,5-DichloroanilineHCID 68320Ethyl 3-bromopropionate

生成物 1

HCID 19978192HCID 19978192、化合物収率 49.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f34c84f955864d789d016137a0f23747
出典データセット
uspto-grants-1997_02
特許番号
US05599813

反応ノート

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