Reaktion #46893

Reaktionsgleichung

HCl

NaH

2,2,2-trifluoro-ethanol

2-Amino-6-fluoro-3-nitro-benzoic acid ethyl ester

→

2-Amino-3-nitro-6-(2,2,2-trifluoro-ethoxy)-benzoic acid ethyl ester

Lösungsmittel

THF

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigemost of the solvent was removed under reduced pressure
2. 2
   workup.ADDITIONThe residue was mixed with 20 mL water
3. 3
   Sonstigethe resulting solid was collected
4. 4
   Waschenwashed with water
5. 5
   SonstigeThe obtained yellow crystalline material was dried under reduced pressure at 35° C

Vorschrift

420 mg NaH (60% suspension in oil) were added to a solution of 2.16 mL (29.8 mmol) 2,2,2-trifluoro-ethanol in 5 mL THF. When the gas evolution ceased, 1.0 g (4.38 mmol) 2-Amino-6-fluoro-3-nitro-benzoic acid ethyl ester was added. The resulting mixture was stirred at 0° C. for 30 minutes and at room temperature for further 30 minutes. To this mixture were added 2 mL of a 6 M aqueous HCl-solution, and most of the solvent was removed under reduced pressure. The residue was mixed with 20 mL water and the resulting solid was collected and washed with water and then hexane. The obtained yellow crystalline material was dried under reduced pressure at 35° C. Yield: 1.22 g.

Quelle