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Triethylamine → Methyl [(5-chloropyridin-2-yl)amino](oxo)acetate

HRID 2104378
ノート
印刷プレビュー

反応式

HRID 2104378 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][N:3]=1.C(N(CC)CC)C.Cl[C:17](=[O:23])[C:18]([O:20][CH2:21]C)=[O:19].C(=O)([O-])O.[Na+]>C(Cl)Cl>[CH3:21][O:20][C:18](=[O:19])[C:17]([NH:1][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][N:3]=1)=[O:23]
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 8471TriethylamineHCID 20884Ethoxalyl chlorideHCID 661742-Amino-5-chloropyridineHCID 516892Sodium Bicarbonate

生成物 1

HCID 44119563Methyl [(5-chloropyridin-2-yl)amino](oxo)acetate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

2-Amino-5-chloropyridine (1.16 g) and triethylamine (1.51 mL) were dissolved in methylene chloride (26 mL), and ethyl chlorooxoacetate (1.10 mL) was added thereto under ice cooling, followed by stirring at room temperature for 14 hours. Saturated aqueous sodium hydrogencarbonate was added to the reaction mixture to partition the mixture, and the organic layer was dried over sodium sulfate anhydrate. The solvent was distilled away under reduced pressure, and the residue was purified by silica gel column chromatography (hexane:ethyl acetate=3:1). The resultant pale-yellow solid was dissolved in methanol (20 mL), and the solution was stirred at 50° C. for 11 hours. The reaction mixture was concentrated under reduced pressure. The precipitated crystals were collected by filtration, and were dried, to thereby give the title compound (0.43 g).

後処理

  1. customto partition the mixture
  2. dry with materialthe organic layer was dried over sodium sulfate anhydrate
  3. distillationThe solvent was distilled away under reduced pressure
  4. customthe residue was purified by silica gel column chromatography (hexane:ethyl acetate=3:1)
  5. dissolutionThe resultant pale-yellow solid was dissolved in methanol (20 mL)
  6. stirringthe solution was stirred at 50° C. for 11 hours
  7. concentrationThe reaction mixture was concentrated under reduced pressure
  8. filtrationThe precipitated crystals were collected by filtration
  9. customwere dried

出典と根拠

ORDレコード
ord-34cc499268d947ba9a6ff01894060f0d
出典データセット
uspto-grants-2009_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07576135B2

反応ノート

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