Water → HCID 68589889, Verbindung

HRID 472753Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 472753
[CH3:1][O:2][C:3](=[O:14])[CH2:4][NH:5][CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[NH2:13].Cl[C:16]([O:19]C(=O)OC(Cl)(Cl)Cl)(Cl)Cl.O>O1CCOCC1>[CH3:1][O:2][C:3](=[O:14])[CH2:4][N:5]1[CH2:6][C:7]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[NH:13][C:16]1=[O:19]

Komponenten

5

Edukt 3

HCID 962WaterHCID 94429TriphosgeneHCID 65440269(2-Amino-benzylamino)-acetic acid methyl ester

Produkt 1

HCID 68589889HCID 68589889, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

(2-Amino-benzylamino)-acetic acid methyl ester (0.50 g, 2 mmol) and bis(trichloromethyl)carbonate (0.54 g, 2 mmol) are dissolved in dioxane (5 ml) and stirred at RT for 24 hours. The reaction mixture is treated with water and extracted with EtOAc, the organic phase is dried over MgSO4, filtered and is concentrated in vacuo. Purification by flash column chromatography on silica, eluting with DCM:MeOH (10:1) affords the title compound. [M+H]+ 221.

Aufarbeitung

  1. extractionextracted with EtOAc
  2. dry with materialthe organic phase is dried over MgSO4
  3. filtrationfiltered
  4. concentrationis concentrated in vacuo
  5. customPurification by flash column chromatography on silica
  6. washeluting with DCM:MeOH (10:1)

Quellen und Nachweise

ORD-Eintrag
ord-ff2e07721b4a48c8a7fdcf452ab50b8a
Quelldatensatz
uspto-grants-2014_01
Patentnummer
US08633211B2

Notizen zur Reaktion

Wird geladen…