Benzaldehyde → Ethyl 2-(benzylideneamino)acetate

HRID 1263166

Reaktionsgleichung

Reaktionsgleichung von HRID 1263166
Cl.[NH2:2][CH2:3][C:4]([O:6][CH2:7][CH3:8])=[O:5].S([O-])([O-])(=O)=O.[Mg+2].C(N(CC)CC)C.[CH:22](=O)[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1>C(Cl)Cl>[C:4]([CH2:3][N:2]=[CH:22][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)([O:6][CH2:7][CH3:8])=[O:5]

Komponenten

6

Edukt 4

HCID 240BenzaldehydeHCID 8471TriethylamineHCID 24083Sulfuric acid magnesium salt (1:1)HCID 2723640Glycine ethyl ester, hydrochloride

Produkt 1

HCID 357745Ethyl 2-(benzylideneamino)acetate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To ethyl glycinate hydrochloride (36.4 g) suspended in 500 ml methylene chloride were added magnesium sulfate (22 g) and triethylamine (72 ml, 52.4 g). Benzaldehyde (27.6 g) was added dropwise at 15°-20° C. with stirring. The mixture was stirred at room temperature for two hours, filtered and stripped. To the residue was added 300 ml diethylether and 150 ml brine. After separation the organic layer was collected, and the aqueous layer was extracted with 100 ml ether. The organic phases were combined, dried (MgSO4), filtered and stripped to yield the title product as a pale yellow oil.

Aufarbeitung

  1. stirringThe mixture was stirred at room temperature for two hours
  2. filtrationfiltered
  3. additionTo the residue was added 300 ml diethylether and 150 ml brine
  4. customAfter separation the organic layer
  5. customwas collected
  6. extractionthe aqueous layer was extracted with 100 ml ether
  7. dry with materialdried (MgSO4)
  8. filtrationfiltered

Quellen und Nachweise

ORD-Eintrag
ord-aa81e46f05784623b13d2ebc3b0c126b
Quelldatensatz
uspto-grants-1984_06
Patentnummer
US04456467

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