Reaktion #1435742

Reaktionsgleichung

sodium borohydride

2-(3,5-bis-trifluoromethyl-phenyl)-N-[4-(2-formyl-phenyl)-6-(4-methyl-piperazin-1-yl)-pyridin-3-yl]-N-methyl-isobutyramide

→

title compound

Ausbeute 68.2%

2-(3,5-Bis-trifluoromethyl-phenyl)-N-[4-(2-hydroxymethyl-phenyl)-6-(4-methyl-piperazin-1-yl)-pyridin-3-yl]-N-methyl-isobutyramide

Ausbeute 68.2%

Lösungsmittel

brine

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwere added at 0° C
2. 2
   workup.ADDITIONwas added at 0° C
3. 3
   workup.DISTILLATIONMethanol was distilled off
4. 4
   workup.ADDITIONthe residue was diluted with 20 ml ethyl acetate
5. 5
   Waschenwashed with 20 ml brine
6. 6
   TrocknenThe organic layer was dried over sodium sulfate
7. 7
   Einengenconcentrated
8. 8
   Sonstigepurified by flash chromatography

Vorschrift

To a mixture of 15 mg (0.41 mmol) sodium borohydride in 2 ml methanol were added at 0° C. 200 mg (0.338 mmol) 2-(3,5-bis-trifluoromethyl-phenyl)-N-[4-(2-formyl-phenyl)-6-(4-methyl-piperazin-1-yl)-pyridin-3-yl]-N-methyl-isobutyramide. After stirring at 0° C. for 1 h 1 ml brine was added at 0° C. The mixture was stirred for 30 min. Methanol was distilled off and the residue was diluted with 20 ml ethyl acetate and washed with 20 ml brine. The organic layer was dried over sodium sulfate, concentrated and purified by flash chromatography to give 137 mg (68%) of the title compound as a light brown solid.

Quelle