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

HRID 1392755
ノート
印刷プレビュー

反応式

HRID 1392755 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-ca39890d42df4debaa3da04cf2d7f8ec
出典データセット
uspto-grants-2008_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07342014B2

反応ノート

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