Iodine → Benzyl [2-(5-ethyloxazol-2-yl)ethyl]carbamate

HRID 1804554Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1804554
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.II.C(N(CC)CC)C.O=[C:30]([CH2:48][CH3:49])[CH2:31][NH:32][C:33]([CH2:35][CH2:36][NH:37][C:38](=[O:47])[O:39][CH2:40][C:41]1[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=1)=[O:34]>ClCCl>[CH2:48]([C:30]1[O:34][C:33]([CH2:35][CH2:36][NH:37][C:38](=[O:47])[O:39][CH2:40][C:41]2[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=2)=[N:32][CH:31]=1)[CH3:49]

Komponenten

6

Edukt 4

HCID 807IodineHCID 8471TriethylamineHCID 11776TriphenylphosphineHCID 57637089Benzyl [2-(2-oxobutylcarbamoyl)ethyl]carbamate

Produkt 1

HCID 57636953Benzyl [2-(5-ethyloxazol-2-yl)ethyl]carbamate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

23.07 g (49.60 mmol) PS-triphenylphosphine are suspended in 200 ml dichloromethane, 12.65 g (49.82 mmol) iodine are added. The mixture is stirred for 0.1 hours at ambient temperature, then 13.80 ml (99.28 mmol) triethylamine are added dropwise. 5.80 g (19.84 mmol) benzyl [2-(2-oxo-butylcarbamoyl)-ethyl]-carbamate dissolved in 150 ml dichloromethane are added. The reaction mixture is stirred for 72 hours at ambient temperature, then the precipitate is filtered off. The filtrate is extracted with water, the organic phase is dried and evaporated to dryness.

Aufarbeitung

  1. additionare added
  2. stirringThe reaction mixture is stirred for 72 hours at ambient temperature
  3. filtrationthe precipitate is filtered off
  4. extractionThe filtrate is extracted with water
  5. customthe organic phase is dried
  6. customevaporated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-344c509a61b94b95b2a986106514681b
Quelldatensatz
uspto-grants-2013_01
Patentnummer
US08354418B2

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