反応 #1897

反応方程式

2-amino-5-bromophenyl-2-pyridylketone

methanol

sodium borohydride

→

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

反応条件

後処理

1. 1
   その他The solvent methanol was evaporated off under reduced pressure
2. 2
   workup.ADDITIONThe residue was treated with an aqueous solution of hydrochloric acid
3. 3
   抽出extracted with ethyl acetate
4. 4
   洗浄The ethyl acetate layer was washed with water
5. 5
   乾燥dried over anhydrous magnesium sulfate
6. 6
   濃縮concentrated under reduced pressure
7. 7
   その他The residue was purified by silica gel column chromatography (eluent, hexane:ethyl acetate=2:1)

実験手順

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.

出典