Ethylamine → HCID 7038767, Verbindung

HRID 247514Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 247514
[NH:1]([C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])[C@@H:2]([C:7]([OH:9])=O)[CH2:3][CH:4]([CH3:6])[CH3:5].O.C[N:19]1CCO[CH2:21][CH2:20]1.C(Cl)(=O)OCC.C(N)C>C1COCC1>[NH:1]([C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])[C@@H:2]([C:7]([NH:19][CH2:20][CH3:21])=[O:9])[CH2:3][CH:4]([CH3:5])[CH3:6]

Komponenten

6

Edukt 4

HCID 6341EthylamineHCID 79724-MethylmorpholineHCID 10928Ethyl chloroformateHCID 2724763D-Leucine, N-[(1,1-dimethylethoxy)carbonyl]-, monohydrate

Produkt 1

HCID 7038767HCID 7038767, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Reaktionsbedingungen

Temperatur
-20 °C

Versuchsvorschrift

25 g of Boc-D-Leu-OH.H2O was dissolved in 200 ml of THF. The solution was cooled to -20° C. 11 ml of N-methylmorpholine and 9.56 ml of ethyl chlorocarbonate were added to the solution. After 5 min, 12.9 g of a 70% aqueous ethylamine solution was added thereto and the mixture was stirred at about -5° C. for 2 h. After concentration, the residue was dissolved in ethyl acetate and washed with an aqueous NaHCO3 solution and water successively. After concentration to dryness, 24.5 g of Boc-D-Leu-NHC2H5 was obtained.

Aufarbeitung

  1. concentrationAfter concentration
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washwashed with an aqueous NaHCO3 solution and water successively
  4. concentrationAfter concentration to dryness

Quellen und Nachweise

ORD-Eintrag
ord-de080da5d0764931831bd1dba3bd98c8
Quelldatensatz
uspto-grants-1987_11
Patentnummer
US04707468

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