Reaktion #3355

Reaktionsgleichung

2,2'-dithiobisbenzoyl chloride

4-[(acetylamino) sulfonyl]aniline

→

2,2'-Dithiobis[N-[4-[(acetylamino)sulfonyl]phenyl]benzamide]

Ausbeute 8.9%

title compound

Ausbeute 8.9%

Lösungsmittel

dichloromethane

pyridine

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe compound was prepared
2. 2
   SonstigeThe crude product was purified on a silica gel column
3. 3
   Einengenconcentrated in vacuo
4. 4
   Sonstigethe solid was crystallized from ethanol/water (1:1 v/v)

Vorschrift

The compound was prepared according to the general method of Preparation 9 using 2,2'-dithiobisbenzoyl chloride (3.0 g, 8.0 mmol) in 30 mL of dichloromethane and 4-[(acetylamino) sulfonyl]aniline (5.6 g, 26.0 mmol) in 100 mL of pyridine. The crude product was purified on a silica gel column using chloroform/methanol (1:1 v/v) as the mobile phase. The pure fractions were pooled, concentrated in vacuo, and the solid was crystallized from ethanol/water (1:1 v/v) to yield 0.5 g of the title compound, mp 180°-182° C.

Quelle