Reaktion #217808

Reaktionsgleichung

N-(3-pentafluorosulfanylphenyl)methanesulfonamide

methyl 4-fluoro-5-methanesulfonyl-2-methylbenzoate

→

resinous solid

Ausbeute 25.6%

Methyl 5-methanesulfonyl-2-methyl-4-(3-pentafluorosulfanylphenyl-amino)benzoate

Ausbeute 25.6%

Lösungsmittel

EA

NMP

Reaktionsbedingungen

Aufarbeitung

1. 1
   Waschenwashed firstly 3 times with 30 ml of a saturated aqueous Na2CO3 solution each time
2. 2
   TrocknenThe residue after drying over MgSO4 and removal of the solvent in vacuo
3. 3
   Sonstigewas chromatographed on silica gel with DIP

Vorschrift

1.0 g of N-(3-pentafluorosulfanylphenyl)methanesulfonamide, 0.8 g of methyl 4-fluoro-5-methanesulfonyl-2-methylbenzoate and 1.4 ml of TBTMG were dissolved in 10 ml of NMP (anhydrous) and stirred at 150° C. for 7 h. The mixture was then diluted with 100 ml of EA and washed firstly 3 times with 30 ml of a saturated aqueous Na2CO3 solution each time and then 3 times with 30 ml of a saturated aqueous NaHSO4 solution each time. The residue after drying over MgSO4 and removal of the solvent in vacuo was chromatographed on silica gel with DIP. 370 mg of a resinous solid were obtained.

Quelle