Monoperoxyphthalic Acid Magnesium Salt → HCID 86613450, Verbindung

HRID 507827

Reaktionsgleichung

Reaktionsgleichung von HRID 507827
[CH3:1][O:2][CH2:3][CH2:4][CH2:5][O:6][C:7]1[CH:32]=[CH:31][CH:30]=[CH:29][C:8]=1[C:9]([NH:11][CH2:12][C@H:13]([CH:26]([CH3:28])[CH3:27])[CH2:14][C@H:15]([NH:18][C:19](=[O:25])[O:20][C:21]([CH3:24])([CH3:23])[CH3:22])[CH:16]=[CH2:17])=[O:10].C(O[O-])(=O)C1C(=CC=CC=1)C([O-])=[O:37].[Mg+2]>CO>[CH3:1][O:2][CH2:3][CH2:4][CH2:5][O:6][C:7]1[CH:32]=[CH:31][CH:30]=[CH:29][C:8]=1[C:9]([NH:11][CH2:12][C@H:13]([CH:26]([CH3:27])[CH3:28])[CH2:14][C@H:15]([NH:18][C:19](=[O:25])[O:20][C:21]([CH3:23])([CH3:24])[CH3:22])[C@@H:16]1[CH2:17][O:37]1)=[O:10]

Komponenten

4

Edukt 2

HCID 10130449Monoperoxyphthalic Acid Magnesium SaltHCID 86613451HCID 86613451, Verbindung

Produkt 1

HCID 86613450HCID 86613450, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

The solution of 1.48 g of tert-butyl (3(S)-{[2-(3-methoxypropoxy)benzoylamino]methyl}-4-methyl-1(S)-vinylpentyl)carbamate in 30 ml of methanol is admixed with 7.81 g of magnesium monoperoxyphthalate and stirred over 72 hours. The reaction mixture is poured onto water and extracted with tert-butyl methyl ether (2×). The combined organic phases are washed with water and brine, dried over sodium sulphate and concentrated by evaporation. The title compound is obtained from the residue by means of flash chromatography (SiO2 60F) as a yellowish oil. Rf=0.30 (1:1 EtOAc-heptane, run 2×); Rt=18.64 (gradient II).

Aufarbeitung

  1. additionThe reaction mixture is poured onto water
  2. extractionextracted with tert-butyl methyl ether (2×)
  3. washThe combined organic phases are washed with water and brine
  4. dry with materialdried over sodium sulphate
  5. concentrationconcentrated by evaporation

Quellen und Nachweise

ORD-Eintrag
ord-1ed91074025e403d8d8a96b4629661c0
Quelldatensatz
uspto-grants-2010_08
Patentnummer
US07786307B2

Verknüpfte Notizen

Wird geladen…