반응 #1897

반응 방정식

2-amino-5-bromophenyl-2-pyridylketone

methanol

sodium borohydride

→

2-amino-5-bromo-α-(2-pyridyl)benzyl alcohol

반응 조건

후처리

1. 1
   기타The solvent methanol was evaporated off under reduced pressure
2. 2
   workup.ADDITIONThe residue was treated with an aqueous solution of hydrochloric acid
3. 3
   추출extracted with ethyl acetate
4. 4
   세척The ethyl acetate layer was washed with water
5. 5
   건조dried over anhydrous magnesium sulfate
6. 6
   농축concentrated under reduced pressure
7. 7
   기타The residue was purified by silica gel column chromatography (eluent, hexane:ethyl acetate=2:1)

실험 절차

In 100 ml of methanol was dissolved 10 g of 2-amino-5-bromophenyl-2-pyridylketone. To the solution was added 1.7 g of sodium borohydride and stirred for 30 minutes. The solvent methanol was evaporated off under reduced pressure. The residue was treated with an aqueous solution of hydrochloric acid. The decomposed residue was then neutralized with 200 ml of a sodium bicarbonate aqueous solution, and extracted with ethyl acetate. The ethyl acetate layer was washed with water, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent, hexane:ethyl acetate=2:1) to give 2-amino-5-bromo-α-(2-pyridyl)benzyl alcohol (9.0 g) as prisms, m.p. 104°-105° C.

출처