Reaktion #54829

Reaktionsgleichung

hydrochloric acid

ethyl 3-amino-4-cyclohexylphenylglyoxylate

hydrochloric acid

sodium nitrite

→

3-hydroxy-4-cyclohexylphenylglyoxylic acid

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONis added dropwise a solution of 1.2 g
2. 2
   workup.ADDITIONThe reaction mixture is then poured onto ice water
3. 3
   Extraktionextracted with chloroform
4. 4
   Trocknendried over sodium sulfate
5. 5
   Einengenconcentrated in vacuo
6. 6
   SonstigeThe residue is crystallized

Vorschrift

To 4.5 g. of ethyl 3-amino-4-cyclohexylphenylglyoxylate suspension in 125 ml. of 80% hydrochloric acid and cooled to 0° C. is added dropwise a solution of 1.2 g. of sodium nitrite in 15 ml. of water. After about 10 min., 200 ml. of 50% hydrochloric acid is added portion wise and stirred for 15 hours. The reaction mixture is then poured onto ice water and extracted with chloroform, dried over sodium sulfate and concentrated in vacuo. The residue is crystallized to obtain 3-hydroxy-4-cyclohexylphenylglyoxylic acid.

Quelle