تفاعل #1435742

معادلة التفاعل

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

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title compound

المردود 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

المردود 68.2%

المذيبات

brine

methanol

ظروف التفاعل

المعالجة

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
   غسيلwashed with 20 ml brine
6. 6
   تجفيفThe organic layer was dried over sodium sulfate
7. 7
   تركيزconcentrated
8. 8
   أخرىpurified by flash chromatography

الإجراء التجريبي

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.

المصدر