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Benzylamine → N-Benzyl 2-(Carbobenzyloxyamino)-3-Methoxypropionamide

HRID 965202
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 965202
[C:1]([NH:11][CH:12]([CH2:16][O:17][CH3:18])[C:13]([OH:15])=O)([O:3][CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)=[O:2].CN1CCOCC1.ClC(OCC(C)C)=O.[CH2:34]([NH2:41])[C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1>>[CH2:34]([NH:41][C:13](=[O:15])[CH:12]([NH:11][C:1]([O:3][CH2:4][C:5]1[CH:6]=[CH:7][CH:8]=[CH:9][CH:10]=1)=[O:2])[CH2:16][O:17][CH3:18])[C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 4

HCID 7504BenzylamineHCID 79724-MethylmorpholineHCID 62365Isobutyl chloroformateHCID 123447572-([(Benzyloxy)carbonyl]amino)-3-methoxypropanoic acid

Produkt 1

HCID 23509063N-Benzyl 2-(Carbobenzyloxyamino)-3-Methoxypropionamide

Versuchsvorschrift

A solution of 11 (0.52 g, 2.04 mmol) in dry tetrahdrofuran (10 mL) was cooled to -78° C. in a dry ice-acetone bath under a N2 atmosphere. To this was added via a dry syringe 4-methylmorpholine (0.34 mL, 3.06 mmol). After stirring for 5 minutes, isobutyl chloroformate (0.4 mL, 3.06 mmol) was added via dry syringe and then the mixture stirred for 5 minutes. This was followed by the addition of benzylamine (0.32 mL, 3.06 mmol). After stirring at -78° C. for 5 minutes, the reaction was allowed to warm to room temperature, and stirring was continued at room temperature (30 min). The hydrochloride salt of 4-methyl morpholine was removed from the reaction by filtration. The clear filtrate was evaporated in vacuo and the residue was triturated with ethyl ether (5.0 mL). The white crystalline product obtained was isolated by filtration after washing with small amounts of ether and air-dried (0.55 g, 78%): mp 112°-114° C., Rf 0.6 (10% MeOH/CHCl3)

Aufarbeitung

  1. customvia dry syringe
  2. stirringthe mixture stirred for 5 minutes
  3. stirringAfter stirring at -78° C. for 5 minutes
  4. stirringstirring
  5. customwas continued at room temperature
  6. custom(30 min)
  7. customThe hydrochloride salt of 4-methyl morpholine was removed from the reaction by filtration
  8. customThe clear filtrate was evaporated in vacuo
  9. customthe residue was triturated with ethyl ether (5.0 mL)
  10. customThe white crystalline product obtained
  11. customwas isolated by filtration
  12. washafter washing with small amounts of ether
  13. customair-dried (0.55 g, 78%)

Quellen und Nachweise

ORD-Eintrag
ord-9cf2a8e9aca44d89ac53d297b242cec3
Quelldatensatz
uspto-grants-1998_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05773475

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