Reaktion #3876

Reaktionsgleichung

3-[2-[4-(4-trifluoromethylphenoxy)phenoxy]-propionyl]-thiocarbazic acid-O-ethyl ester

→

compound

Ausbeute 57.4%

2-ethoxy-5-[1-[4-(4-trifluoromethylphenoxy)phenoxy]-ethyl]-1,3,4-thiadiazole

Ausbeute 57.4%

Lösungsmittel

sulfuric acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwas added
2. 2
   workup.STIRRINGAfter stirring at the same temperature for 10 minutes
3. 3
   Extraktionby extracting with ethyl acetate
4. 4
   WaschenThe resulting ethyl acetate layer was washed with water
5. 5
   Trocknendried over anhydrous sodium sulfate
6. 6
   Einengenconcentrated
7. 7
   SonstigeThe residue was purified by chromatography on silica gel

Vorschrift

To 10 ml of concentrated sulfuric acid cooled to -5° C. was added, with stirring, 2.0 g of 3-[2-[4-(4-trifluoromethylphenoxy)phenoxy]-propionyl]-thiocarbazic acid-O-ethyl ester gradually. After stirring at the same temperature for 10 minutes, the reaction mixture was poured over 100 g of ice followed by extracting with ethyl acetate. The resulting ethyl acetate layer was washed with water, dried over anhydrous sodium sulfate, and concentrated. The residue was purified by chromatography on silica gel to obtain 1.1 g of the compound No. 5 described in Table 1.

Quelle