2-[4-(4-Bromophenoxymethyl)-2,5-dioxo-imidazolidin-1-yl]-3-methyl-butyric acid methyl ester → HCID 66660886, Verbindung

HRID 2197271

Reaktionsgleichung

Reaktionsgleichung von HRID 2197271
C[O:2][C:3](=[O:29])[CH:4]([NH:8][C:9](=[O:28])[CH:10]([NH:20][C:21](OC(C)(C)C)=[O:22])[CH2:11][O:12][C:13]1[CH:18]=[CH:17][C:16]([Br:19])=[CH:15][CH:14]=1)[CH:5]([CH3:7])[CH3:6].COC(=O)C(N1C(=O)C(COC2C=CC(Br)=CC=2)NC1=O)C(C)C>Cl>[Br:19][C:16]1[CH:17]=[CH:18][C:13]([O:12][CH2:11][CH:10]2[C:9](=[O:28])[N:8]([CH:4]([CH:5]([CH3:7])[CH3:6])[C:3]([OH:2])=[O:29])[C:21](=[O:22])[NH:20]2)=[CH:14][CH:15]=1

Komponenten

4

Edukt 2

HCID 666606712-[4-(4-Bromophenoxymethyl)-2,5-dioxo-imidazolidin-1-yl]-3-methyl-butyric acid methyl esterHCID 666609032-[3-(4-Bromophenoxy)-2-tert-butoxycarbonylamino-propionylamino]-3-methyl-butyric acid methyl ester

Produkt 1

HCID 66660886HCID 66660886, VerbindungAusbeute 41 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 313Hydrochloric AcidLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

A mixture of the compound obtained in step g above (22g) (759 mg, 1.907 mmol) and 3 N HCl (20 mL) was stirred at 80° C. for 2 h. The reaction mixture was cooled down and then extracted with EtOAc. The combined organic layers were dried and concentrated; the crude product was purified by silica gel column chromatography which gave the title compound as colorless oil (300 mg, 41%).

Aufarbeitung

  1. temperatureThe reaction mixture was cooled down
  2. extractionextracted with EtOAc
  3. customThe combined organic layers were dried
  4. concentrationconcentrated
  5. customthe crude product was purified by silica gel column chromatography which

Quellen und Nachweise

ORD-Eintrag
ord-98db85b568764f85b90ed13c5b86b72e
Quelldatensatz
uspto-grants-2012_12
Patentnummer
US08338471B2

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