反応 #73935

反応方程式

2-((2,4-dichlorobenzyl)(methyl)amino)-1-phenylethanone

NaBH4

→

title compound

収率 79.0%

2-((2,4-dichlorobenzyl)(methyl)amino)-1-phenylethanol

収率 79.0%

溶媒

methanol

反応条件

後処理

1. 1
   その他Into a 250 ml 3-necked roundbottom flask purged
2. 2
   温度maintained with an inert atmosphere of nitrogen
3. 3
   その他The reaction was then quenched by the addition of 20 mL of acetone
4. 4
   濃縮The resulting mixture was concentrated under vacuum

実験手順

Into a 250 ml 3-necked roundbottom flask purged and maintained with an inert atmosphere of nitrogen, was placed a solution of 2-((2,4-dichlorobenzyl)(methyl)amino)-1-phenylethanone (4.3 g, 14.01 mmol, 1.00 equiv) in methanol (50 mL). This was followed by the addition of NaBH4 (1.5 g, 39.47 mmol, 2.82 equiv) in several batches at 0° C. The resulting solution was stirred for 30 min at 0° C. in a water/ice bath. The reaction was then quenched by the addition of 20 mL of acetone. The resulting mixture was concentrated under vacuum. The residue was applied onto a silica gel column with ethyl acetate/petroleum ether (1:80-1:20). This resulted in 3.4 g (79%) of the title compound as a white solid.

出典