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Phenoxyethanol → HCID 15670239, Verbindung

HRID 248698
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 248698
[C:1]([S:4][CH2:5][CH:6]([CH2:22][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)[C:7]([NH:9][C:10]1[CH:11]=[C:12]([CH:19]=[CH:20][CH:21]=1)[C:13]([O:15][CH2:16][C:17]#N)=[O:14])=[O:8])(=[O:3])[CH3:2].[O:29](CCO)[C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1>CN(C)C1C=CN=CC=1.C(N(CC)CC)C>[C:1]([S:4][CH2:5][CH:6]([CH2:22][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)[C:7]([NH:9][C:10]1[CH:11]=[C:12]([CH:19]=[CH:20][CH:21]=1)[C:13]([O:15][CH2:16][CH2:17][O:29][C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1)=[O:14])=[O:8])(=[O:3])[CH3:2]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 2

HCID 31236PhenoxyethanolHCID 15670238HCID 15670238, Verbindung

Produkt 1

HCID 15670239HCID 15670239, VerbindungAusbeute 51,9 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 142844-(Dimethylamino)pyridineKatalysatorHCID 8471TriethylamineLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

Cyanomethyl 3-[(2 acetylthiomethyl-3-phenylpropionyl)amino]benzoate (compound of Example 116) (4 g), 2-phenoxyethanol (3 g), 4-dimethylaminopyridine (0.1 g) and triethylamine (2 g) are mixed, and the mixture is stirred at 60° C. for 15 hours and extracted with ethyl acetate (50 ml). The extract is washed with 10% hydrochloric acid and water, and ethyl acetate is distilled off under reduced pressure. The residue is dissolved in 50% aqueous acetonitrile and purified by a column chromatography using Diaion HP-20 (eluant, water-acetonitrile). The fractions containing the desired compound are collected, and acetonitrile is distilled off under reduced pressure. The aqueous solution is extracted with ethyl acetate (100 ml). The extract is dried over anhydrous magnesium sulfate, and ethyl acetate is distilled off under reduced pressure to give the title compound (2.5 g).

Aufarbeitung

  1. extractionextracted with ethyl acetate (50 ml)
  2. washThe extract is washed with 10% hydrochloric acid and water, and ethyl acetate
  3. distillationis distilled off under reduced pressure
  4. dissolutionThe residue is dissolved in 50% aqueous acetonitrile
  5. custompurified by a column chromatography
  6. additionThe fractions containing the desired compound
  7. customare collected
  8. distillationacetonitrile is distilled off under reduced pressure
  9. extractionThe aqueous solution is extracted with ethyl acetate (100 ml)
  10. dry with materialThe extract is dried over anhydrous magnesium sulfate, and ethyl acetate
  11. distillationis distilled off under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-a9bfba8f528c4d658a91749fd406923a
Quelldatensatz
uspto-grants-1993_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05210266

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