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Trifluoroacetic acid → 2-aminoethyl acetate TFA-salt

HRID 1349005
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1349005
C([CH:8]([CH2:10][NH2:11])O)(OC(C)(C)C)=O.[C:12]([OH:18])([C:14]([F:17])([F:16])[F:15])=[O:13]>C(Cl)Cl>[OH:18][C:12]([C:14]([F:17])([F:16])[F:15])=[O:13].[C:12]([O:18][CH2:8][CH2:10][NH2:11])(=[O:13])[CH3:14]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 6422Trifluoroacetic acidHCID 22707757Propanoic acid, 3-amino-2-hydroxy-, 1,1-dimethylethyl ester

Produkt 1

HCID 873085332-aminoethyl acetate TFA-salt

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A solution was made containing ethanolamine (36.5 ml, 0.6 mol) in chloroform (1000 ml). The Boc2O (13.1 g, 60 mmol) dissolved in chloroform (600 ml) was slowly added dropwise at 0° C. over a 6-hours period (the temperature was maintained all over this period). The reaction was allowed to reach room temperature and was stirred overnight. The organic layer was washed with water (2×500 ml), brine and dried over magnesium sulfate before being concentrated in vacuo. The desired product (9.5 g,>95%) was isolated as a colourless oil and was used without further purification. A solution was made containing the Boc-ethanolamine (1.92 g, 12 mmol) with potassium carbonate (5 g, 36 mmol) in DCM (40 ml). Acetyl chloride (30 ml, 0.42 mol) was added and the reaction stirred for 6 hours at room temperature. The excess of acetyl chloride was removed in vacuo and the crude dissolved in DCM (100 ml). The organic layer was washed with water (50 ml), brine and dried over magnesium sulfate before being concentrated in vacuo. The desired product (1.86 g, 77%) was isolated as a colourless oil and was used without further purification. A solution was made containing the O-acyl, Boc-ethanolamine (1.65 g, 8.1 mmol) in DCM (20 ml) and TFA (20 ml) was added. After one hour at room temperature, the solvent was removed in vacuo. The crude was concentrated from methanol (2–3 times) and from DCM (2–3 times) to give the expected compound (1.75 g, quant.) as an oil used without further purification.

Aufarbeitung

  1. customwas used without further purification
  2. additionwas added
  3. customthe solvent was removed in vacuo
  4. concentrationThe crude was concentrated from methanol (2–3 times) and from DCM (2–3 times)

Quellen und Nachweise

ORD-Eintrag
ord-0a83f236aca54e71ab2448e5afa22057
Quelldatensatz
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07211601B2

Notizen zur Reaktion

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