Reaktion #520090

Reaktionsgleichung

chlorosulfonic acid

4-(4-methoxy-phenoxy)-3,5-dichloro-nitrobenzene

→

title compound

5-(2,6-Dichloro-4-nitro-phenoxy)-2-methoxy-benzenesulfonyl chloride

Lösungsmittel

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.WAITat RT for 2.5 h
2. 2
   Extraktionthe product was extracted with EtOAc (3×50 mL)
3. 3
   SonstigeThe combined organic extracts were dried
4. 4
   Einengenconcentrated

Vorschrift

To cooled chlorosulfonic acid (2.0 mL) at 0° C. was added 4-(4-methoxy-phenoxy)-3,5-dichloro-nitrobenzene (700 mg, 2.2 mmol) in several portions. The resulting mixture was stirred at 0° C. for 5 min, then at RT for 2.5 h. The solution was added dropwise to ice water (40 mL) and the product was extracted with EtOAc (3×50 mL). The combined organic extracts were dried and concentrated to yield the title compound of Step A (920 mg) as a crude product which was used in the next step without purification. MS (APCl−) Calc.: 410.9, Found: 392.1 (M−1-Cl+OH, sulfonic acid).

Quelle