Reaktion #54831

Reaktionsgleichung

ethyl 3-amino-4-cyclohexylphenylglyoxylate

hydrobromic acid

hydrobromic acid

sodium nitrite

→

3-bromo-4-cyclohexylphenylglyoxylic acid

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONis added dropwise a solution of 2.34 g
2. 2
   workup.ADDITIONTo this mixture is added a solution of 20 g
3. 3
   workup.ADDITIONThe reaction mixture is then poured onto ice water
4. 4
   Extraktionextracted with chloroform
5. 5
   Trocknendried over sodium sulfate
6. 6
   Einengenconcentrated in vacuo
7. 7
   SonstigeThe residue is then crystallized

Vorschrift

To 11.1 g. (0.044 moles) of ethyl 3-amino-4-cyclohexylphenylglyoxylate suspension in 225 ml. of 40% hydrobromic acid and cooled to 0° C. is added dropwise a solution of 2.34 g. of sodium nitrite in 30 ml. of water. To this mixture is added a solution of 20 g. of cuprous bromide in 350 ml. of 40% hydrobromic acid added portion wise and stirred for 15 hours. The reaction mixture is then poured onto ice water, extracted with chloroform, dried over sodium sulfate and concentrated in vacuo. The residue is then crystallized to obtain 3-bromo-4-cyclohexylphenylglyoxylic acid.

Quelle