反応 #71416

反応方程式

LiAlH4

4-(4-methoxybenzyl)-3,3-dimethyl-piperazin-2-one

→

title compound

収率 92.3%

1-(4-Methoxy-benzyl)-2,2-dimethyl-piperazine

収率 92.3%

溶媒

THF

反応条件

後処理

1. 1
   その他quenched by sequential addition of H2O (1 mL), 1 N NaOH (1 mL) and H2O (3 mL)
2. 2
   ろ過filtered through a pad of celite
3. 3
   濃縮concentrated

実験手順

LiAlH4 (1M in THF, 27.8 mL, 27.8 mmol, 1.5 equiv) was added to a solution of 4-(4-methoxybenzyl)-3,3-dimethyl-piperazin-2-one (Step 108.3) (4.6 g, 18.5 mmol) in THF (100 mL) at 50° C., under an argon atmosphere. The resulting mixture was stirred for 2 h at 50° C., quenched by sequential addition of H2O (1 mL), 1 N NaOH (1 mL) and H2O (3 mL), filtered through a pad of celite and concentrated to afford 4.0 g of the title compound as a white solid: ESI-MS: 235.2 [M+H]+.

出典