Triethylamine → HCID 54241030, Verbindung

HRID 377574

Reaktionsgleichung

Reaktionsgleichung von HRID 377574
[C:1]([SiH:5]([CH3:7])[CH3:6])([CH3:4])([CH3:3])[CH3:2].C(N(CC)CC)C.[C:15]([O:18][CH2:19][C:20]1[O:25][CH2:24][N:23]([C:26]([CH3:38])([CH3:37])[C:27]([O:29]CC2C=CC=CC=2)=[O:28])[C:22](=[O:39])[C:21]=1[C:40]1[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=1)(=[O:17])[CH3:16]>ClCCl.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[C:15]([O:18][CH2:19][C:20]1[O:25][CH2:24][N:23]([C:26]([CH3:38])([CH3:37])[C:27]([O:29][Si:5]([C:1]([CH3:4])([CH3:3])[CH3:2])([CH3:7])[CH3:6])=[O:28])[C:22](=[O:39])[C:21]=1[C:40]1[CH:41]=[CH:42][CH:43]=[CH:44][CH:45]=1)(=[O:17])[CH3:16]

Komponenten

6

Edukt 3

HCID 8471TriethylamineHCID 5072427tert-ButyldimethylsilaneHCID 19354621HCID 19354621, Verbindung

Produkt 1

HCID 54241030HCID 54241030, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 167845palladium(II) acetateKatalysatorHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A mixture of palladium (II) acetate (25 mg), tert butyl-dimethylsilane (1.25 ml) and triethylamine (0.05 ml) in dichloromethane was stirred at room temperature under an inert atmosphere for 0.25 hour. A solution of benzyl 2-(6-acetoxymethyl-2,3-dihydro-4-oxo-5-phenyl-4H-1,3-oxazin-3-yl)-2-methylpropanoate (1.0 g) was added and stirring continued for 18 hours. The mixture was filtered (hyflo) and evaporated to give tert butyldimethylsilyl 2-(6-acetoxymethyl-2,3-dihydro-4-oxo-5-phenyl-4H-1,3-oxazin-3-yl)-2-methylpropanoate (0.92 g) as a yellow oil, NMR (CDCl3)δ 0.25(s,9H), 1.5(s,6H), 2.0(s,3H), 4.5(s,2H), 5.2(s,2H), 7.0-7.3(m,5H).

Aufarbeitung

  1. stirringstirring
  2. waitcontinued for 18 hours
  3. filtrationThe mixture was filtered (hyflo)
  4. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-76627ef6a68c4b3180a02e79451d048d
Quelldatensatz
uspto-grants-2000_02
Patentnummer
US06028032

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