反応 #338647

反応方程式

4-(3-oxa-1-azaspiro[4.5]dec-1-en-2-yl)phenol

1-bromo-3-chloro-2-methylpropane

potassium carbonate

→

2-[4-(3-chloro-2-methylpropoxy)phenyl]-3-oxa-1-azaspiro[4.5]dec-1-ene

収率 100.0%

溶媒

acetone

反応条件

後処理

1. 1
   温度at reflux for 13 days
2. 2
   濃縮The mixture is concentrated
3. 3
   洗浄washed twice with a saturated aqueous solution of ammonium chloride
4. 4
   乾燥The organic layer is dried over magnesium sulfate
5. 5
   その他the solvent is removed under reduced pressure

実験手順

To a solution of 4-(3-oxa-1-azaspiro[4.5]dec-1-en-2-yl)phenol ax8 (0.5 g, 2.16 mmol, 1 eq) in acetone (30 ml) is added 1-bromo-3-chloro-2-methylpropane (0.25 ml, 2.16 mmol, 1 eq) and potassium carbonate (0.6 g, 4.32 mmol, 2 eq). The mixture is stirred at reflux for 13 days. The mixture is concentrated, taken up in dichloromethane and washed twice with a saturated aqueous solution of ammonium chloride. The organic layer is dried over magnesium sulfate and the solvent is removed under reduced pressure to afford 0.7 g of 2-[4-(3-chloro-2-methylpropoxy)phenyl]-3-oxa-1-azaspiro[4.5]dec-1-ene ax64 as a colorless oil. This crude product is used in the next step without further purification.

出典