反应 #1897

反应方程式

2-amino-5-bromophenyl-2-pyridylketone

methanol

sodium borohydride

→

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

反应条件

后处理

1. 1
   其他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
   萃取extracted with ethyl acetate
4. 4
   洗涤The ethyl acetate layer was washed with water
5. 5
   干燥dried over anhydrous magnesium sulfate
6. 6
   浓缩concentrated under reduced pressure
7. 7
   其他The residue was purified by silica gel column chromatography (eluent, hexane:ethyl acetate=2:1)

实验过程

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.

来源