Hexamethyldisilazane → HCID 54579443, Verbindung

HRID 75496

Reaktionsgleichung

Reaktionsgleichung von HRID 75496
S([O-])([O-])(=O)=O.[NH4+].[NH4+].[C:8]([NH:11]/[C:12](=[C:18](/[NH:20][CH:21]1[CH2:25][CH2:24][CH2:23][CH2:22]1)\[CH3:19])/[C:13]([O:15][CH2:16][CH3:17])=[O:14])(=O)[CH3:9].C[Si](C)(C)N[Si](C)(C)C>>[CH:21]1([N:20]2[C:18]([CH3:19])=[C:12]([C:13]([O:15][CH2:16][CH3:17])=[O:14])[N:11]=[C:8]2[CH3:9])[CH2:25][CH2:24][CH2:23][CH2:22]1

Komponenten

4

Edukt 3

HCID 13838HexamethyldisilazaneHCID 6097028Ammonium SulfateHCID 54579442(E)-Ethyl 2-acetamido-3-(cyclopentylamino)but-2-enoate2×

Produkt 1

HCID 54579443HCID 54579443, VerbindungAusbeute 71,7 %

Reaktionsbedingungen

Temperatur
150 °C

Versuchsvorschrift

Ammonium sulfate (100 mg) was added to a solution of (E)-ethyl 2-acetamido-3-(cyclopentylamino)but-2-enoate (compound 18, 1.5 g, 5.9 mmol) and hexamethyldisilazane (15 mL) and refluxed overnight at 150° C. The reaction mixture was evaporated and extracted with EA and water. The organic layer was evaporated and the residue was purified with 20% methanol in CH2Cl2 to produce as a light brown solid (1.0 g, 71.4% yield).

Aufarbeitung

  1. customThe reaction mixture was evaporated
  2. extractionextracted with EA and water
  3. customThe organic layer was evaporated
  4. customthe residue was purified with 20% methanol in CH2Cl2

Quellen und Nachweise

ORD-Eintrag
ord-d60c4c69e8b14d838b11d92221ff0a9b
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08835436B2

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