Reaktion #62039

Reaktionsgleichung

potassium tert-butoxide

2-cyanoacetamide

4-(2,5-dichloro-phenoxy)-3-fluoro-phenylisothiocyanate

HCl

→

crude product

Ausbeute 82.5%

2-Cyano-2-[4-(2,5-dichloro-phenoxy)-3-fluoro-phenylthiocarbamoyl]-acetamide

Ausbeute 82.5%

Lösungsmittel

THF

THF

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGAfter 15 min of stirring at 5° C.
2. 2
   Temperaturthis reaction mixture was warmed to room temperature
3. 3
   workup.STIRRINGstirred for another 2 h
4. 4
   workup.STIRRINGwith stirring
5. 5
   FiltrationThe solid was filtered
6. 6
   Waschenwashed with water
7. 7
   SonstigeAfter drying in vacuo

Vorschrift

To a solution of potassium tert-butoxide (0.6 g, 5.36 mmol) in 10 ml of anhydrous THF was added 2-cyanoacetamide (0.45 g, 5.36 mmol) under argon. The mixture was cooled to 5° C. and added dropwise to a solution of 4-(2,5-dichloro-phenoxy)-3-fluoro-phenylisothiocyanate (1.53 g, 4.87 mmol) in 5 ml of dry THF with stirring under argon. After 15 min of stirring at 5° C., this reaction mixture was warmed to room temperature and stirred for another 2 h. The reaction mixture was poured into 200 ml of ice water with stirring and acidified with 10% HCl. The solid was filtered and washed with water. After drying in vacuo, the crude product (1.6 g, 82.5%) was obtained in sufficient purity for the next step.

Quelle