反応 #71419

反応方程式

HCl

{5-[4-(4-methoxy-benzyl)-2,2-dimethyl-piperazin-1-ylmethyl]-pyridin-2-yl}-carbamic acid tert-butyl ester

→

title compound

収率 102.5%

5-[4-(4-Methoxy-benzyl)-2,2-dimethyl-piperazin-1-ylmethyl]-pyridin-2-ylamine

収率 102.5%

溶媒

dioxane

MeOH

反応条件

後処理

1. 1
   温度to cool
2. 2
   その他quenched by addition of a saturated aqueous solution of NaHCO3
3. 3
   抽出extracted with DCM
4. 4
   洗浄The organic layer was washed with a saturated aqueous solution of NaHCO3
5. 5
   乾燥dried (Na2SO4)
6. 6
   ろ過filtered
7. 7
   濃縮concentrated

実験手順

A mixture of {5-[4-(4-methoxy-benzyl)-2,2-dimethyl-piperazin-1-ylmethyl]-pyridin-2-yl}-carbamic acid tert-butyl ester (Step 109.2) (1.88 g, 4.3 mmol), a 4 N solution of HCl in dioxane (25 mL) and MeOH (25 mL) was stirred for 22 h at rt. The reaction mixture was allowed to cool, quenched by addition of a saturated aqueous solution of NaHCO3 and extracted with DCM. The organic layer was washed with a saturated aqueous solution of NaHCO3, dried (Na2SO4), filtered and concentrated to provide 1.5 g of the title compound as a brown solid: ESI-MS: 341.3 [M+H]+; ]+; tR=1.72 min (System 1).

出典