反応 #2006409

反応方程式

NaHCO3

3-aminophenylacetic acid

HCl

→

1

収率 79.0%

Methyl-3-aminophenylacetate

収率 79.0%

溶媒

methanol

反応条件

後処理

1. 1
   その他The solvent was removed under reduced pressure
2. 2
   抽出the aqueous phase was extracted several times with CH2Cl2
3. 3
   乾燥The combined organic extracts were dried over (MgSO4)
4. 4
   その他evaporated
5. 5
   その他The crude mixture was purified by flash chromatography

実験手順

To a solution of 3-aminophenylacetic acid (3 g, 19.85 mmol) in methanol (50 mL) at room temperature was added HCl conc. (37%, 7.5 mL). The mixture was stirred 6 h at room temperature then treated with a saturated aqueous solution of NaHCO3. The solvent was removed under reduced pressure then the aqueous phase was extracted several times with CH2Cl2. The combined organic extracts were dried over (MgSO4) and evaporated. The crude mixture was purified by flash chromatography using hexane/AcOEt (1:1) yielding 1 as a yellow oil (3.06 g, 79%).

出典