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4-Chloroaniline → Ethyl [(4-chlorophenyl)amino](oxo)acetate

HRID 902861
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HRID 902861 반응식
C(N(CC)CC)C.Cl[C:9](=[O:15])[C:10]([O:12][CH2:13][CH3:14])=[O:11].[Cl:16][C:17]1[CH:23]=[CH:22][C:20]([NH2:21])=[CH:19][CH:18]=1.C(=O)([O-])O.[Na+]>C(Cl)Cl>[Cl:16][C:17]1[CH:23]=[CH:22][C:20]([NH:21][C:9](=[O:15])[C:10]([O:12][CH2:13][CH3:14])=[O:11])=[CH:19][CH:18]=1
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참가 물질

6

반응물 4

HCID 78124-ChloroanilineHCID 8471TriethylamineHCID 20884Ethoxalyl chlorideHCID 516892Sodium Bicarbonate

생성물 1

HCID 79380Ethyl [(4-chlorophenyl)amino](oxo)acetate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Triethylamine (1.52 ml) and ethyl chlorooxoacetate (1.11 ml) were successively added to a solution of 4-chloroaniline (1.16 g) in methylene chloride (26 ml), and the mixture was stirred at room temperature for 14 hours. After a saturated aqueous solution of sodium hydrogencarbonate was added to the reaction mixture to conduct liquid separation, the resultant organic layer was successively washed with a 10% aqueous solution of citric acid and saturated aqueous solution of sodium chloride and dried over anhydrous sodium sulfate. After the solvent was concentrated under reduced pressure, hexane was added to the residue to deposit crystals, and the crystals were collected by filtration and dried to obtain the title compound (1.89 g).

후처리

  1. customliquid separation
  2. washthe resultant organic layer was successively washed with a 10% aqueous solution of citric acid and saturated aqueous solution of sodium chloride
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationAfter the solvent was concentrated under reduced pressure, hexane
  5. additionwas added to the residue to deposit crystals
  6. filtrationthe crystals were collected by filtration
  7. customdried

출처 및 근거

ORD 기록
ord-41a8070a5cc34022a31fe0294d322c17
출처 데이터셋
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07365205B2

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