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Benzyl chloroformate → [2-(2-Hydroxy-ethoxy)-ethyl]-carbamic acid benzyl ester

HRID 1383465
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1383465
[NH2:1][CH2:2][CH2:3][O:4][CH2:5][CH2:6][OH:7].[OH-].[Na+].Cl[C:11]([O:13][CH2:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)=[O:12]>O>[CH2:14]([O:13][C:11](=[O:12])[NH:1][CH2:2][CH2:3][O:4][CH2:5][CH2:6][OH:7])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 10387Benzyl chloroformateHCID 13578DiglycolamineHCID 14798Sodium Hydroxide

Produkt 1

HCID 11064482[2-(2-Hydroxy-ethoxy)-ethyl]-carbamic acid benzyl esterAusbeute 67,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

2-(2-Aminoethoxy)ethanol (5.26 g, 50 mmol) and sodium hydroxide (2.1 g, 52.5 mmol) were dissolved in water (200 mL). The resulted solution was cooled in ice bath, followed by the dropwise addition of benzyl chloroformate. After the addition, the reaction mixture was continuously stirred in ice bath for another hour. The desired product was extracted with ethyl acetate (EtOAc, 200 mL). The EtOAc layer was washed with water (3×100 mL) and then dried over anhydrous sodium sulfate. The solvent was removed in vacuo to yield the crude product. The product was further purified by flash column chromatography (SiO2, 1:2 Hexane:EtOAc) to give [2-(2-hydroxy-ethoxy)-ethyl]-carbamic acid benzyl ester as a clear oil (8.07 g, 67.5% yield). 1H-NMR (CDCl3, ppm) 7.35 (m, 5H), 5.34 (b, 1H), 5.10 (s, 2H), 3.71 (m, 2H), 3.56 (m, 4H), 3.41 (m, 2H), 2.20 (b 1H),. ESMS 240.0 (M+1).

Aufarbeitung

  1. temperatureThe resulted solution was cooled in ice bath
  2. additionAfter the addition
  3. extractionThe desired product was extracted with ethyl acetate (EtOAc, 200 mL)
  4. washThe EtOAc layer was washed with water (3×100 mL)
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe solvent was removed in vacuo
  7. customto yield the crude product
  8. customThe product was further purified by flash column chromatography (SiO2, 1:2 Hexane:EtOAc)

Quellen und Nachweise

ORD-Eintrag
ord-32298d0b10014a2aa40f8511e9cc147b
Quelldatensatz
uspto-grants-2001_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06255323B1

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