Reaktion #2320117

Reaktionsgleichung

4-bromo-2-methanesulfonyl-1-methoxy-benzene

piperazine

sodium tert-butoxide

→

1-(3-Methanesulfonyl-4-methoxy-phenyl)-piperazine

Lösungsmittel

Et2O

dioxane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Waschenwashed with brine (15-20 ml)
2. 2
   TrocknenThe organic fraction was dried (MgSO4)
3. 3
   Filtrationfiltered
4. 4
   Sonstigeevaporated to dryness
5. 5
   SonstigeThe crude material was purified by flash chromatography on silica gel

Vorschrift

A mixture of 4-bromo-2-methanesulfonyl-1-methoxy-benzene (0.65 g,), piperazine (0.43 g,), sodium tert-butoxide (0.13 g) BINAP (19 mg) and [Pd2(dba)3 (27 mg) in dioxane (5 ml) was heated under argon at 100° C. for 24 h. After cooling to room temperature, the reaction mixture was taken up in Et2O (40-50 ml) and washed with brine (15-20 ml). The organic fraction was dried (MgSO4), filtered and evaporated to dryness. The crude material was purified by flash chromatography on silica gel using CH2Cl2:MeOH (9:1 (v/v)) Yield 0.14 g: MS m/z (rel. intensity, 70 eV)) 270 (M+, 23), 229 (11), 228 (bp), 148 (7), 56 (17).

Quelle