Reaktion #418375

Reaktionsgleichung

2,3-dichloroquinoxaline

3-methylbenzene sulfonamide

K2CO3

→

title compound

Ausbeute 65.7%

N-(3-chloroquinoxalin-2-yl)-3-methylbenzenesulfonamide

Ausbeute 65.7%

Lösungsmittel

DMA

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe solvent is evaporated to dryness
2. 2
   workup.ADDITIONWater (20 ml) is added
3. 3
   Sonstigethe precipitate formed
4. 4
   Filtrationis filtered off
5. 5
   Waschenwashed with water until neutral, then ACN
6. 6
   Sonstigedried under vacuum at 40° C. overnight

Vorschrift

A suspension of 2,3-dichloroquinoxaline (500 mg; 2.5 mmol; 1 eq), 3-methylbenzene sulfonamide (430.1 mg, 2.5 mmol, 1 eq.), dry K2CO3 (347.2 mg, 2.5 mmol, 1 eq.) in DMA (5 ml) is heated up at 170° C. in the microwave for 30 min under normal absorption. The solvent is evaporated to dryness. Water (20 ml) is added then AcOH until acidic pH. The residual suspension is left at 4° C. for 1 h and the precipitate formed is filtered off, washed with water until neutral, then ACN and dried under vacuum at 40° C. overnight, to afford 548.3 mg (65%) of the title compound. 1H NMR (DMSO-d6) δ 11.53 (brs, 1H), 7.99 (m, 2H), 7.87 (t, J=8.6 Hz, 2H), 7.77 (dt, J=1.5, 7.5 Hz, 1H), 7.67 (t, J=8.0 Hz, 1H), 7.56-7.43 (m, 2H), 2.42 (s, 3H). HPLC (max plot) 99%; Rt 3.70 min. LC/MS: (ES+): 334.2, (ES−): 332.2.

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