Reaktion #162678

Reaktionsgleichung

Ammonium sulfate

(E)-ethyl 2-acetamido-3-(cyclopentylamino)but-2-enoate

compound 18

(E)-ethyl 2-acetamido-3-(cyclopentylamino)but-2-enoate

hexamethyldisilazane

→

solid

Ausbeute 71.7%

Ethyl 1-cyclopentyl-2,5-dimethyl-1H-imidazole-4-carboxylate

Ausbeute 71.7%

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe reaction mixture was evaporated
2. 2
   Extraktionextracted with EA and water
3. 3
   SonstigeThe organic layer was evaporated
4. 4
   Sonstigethe residue was purified with 20% methanol in CH2Cl2

Vorschrift

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).

Quelle