Reaktion #1139799

Reaktionsgleichung

water

1-Fluoro-3-iodo-5-nitrobenzene

potassium carbonate

dimethylamine

→

title compound

Ausbeute 59.0%

3-Iodo-N,N-dimethyl-5-nitroaniline

Ausbeute 59.0%

Lösungsmittel

DMSO

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe vial was sealed under argon
2. 2
   Extraktionextracted with ethyl acetate (3×40 ml)
3. 3
   WaschenThe organic phase was washed with brine (1×100 ml)
4. 4
   Trocknendried over magnesium sulphate
5. 5
   Einengenconcentrated under reduced pressure
6. 6
   SonstigeThe residue was purified
7. 7
   SonstigeSP1® Purification System (0% to 30%, hexane-ethyl acetate)

Vorschrift

1-Fluoro-3-iodo-5-nitrobenzene (500 mg, 1.87 mmol), and potassium carbonate (260 mg, 1.88 mmol) were suspended in DMSO (7 ml) and dimethylamine (2M in THF, 3 ml, 6 mmol) was added. The vial was sealed under argon and stirred for 15 min at 125° C. under microwave conditions. The reaction mixture was poured into 50 ml of water and extracted with ethyl acetate (3×40 ml). The organic phase was washed with brine (1×100 ml), dried over magnesium sulphate and concentrated under reduced pressure. The residue was purified using SP1® Purification System (0% to 30%, hexane-ethyl acetate) to obtain 320 mg (59% yield) of the title compound as a brown solid. Purity 100%.

Quelle