反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 30 °C
PROCEDURE
实验过程
1-Ethyl-1-[2-(trifluoromethyl)-2-propen-1-yl]-1,2,3,4-tetrahydronaphthalene (Intermediate 12) (100 mg, 0.373 mmole), AD-MIX-α (300 mg) and AD-MIX-β (300 mg) in t-butanol (2 ml) and water (2 ml) were stirred at room temperature. After 1 hour further AD-MIX-α (600 mg) and AD-MIX-β (600 mg) were added and the mixture was heated to 30° C. for 18 h. Sodium sulphite (2 g) was added together with water (5 ml) then stirred for 10 min. Extraction of the mixture with ethyl acetate (3×20 ml) followed by washing of the extract with 2M HCl (x2), 2M NaOH and evaporation of volatiles in vacuo gave a crude product. After purification (silica SPE, 85:15 cyclohexane:ethyl acetate) the title compound was obtained (30 mg, 27%).
WORKUP
后处理
- extractionExtraction of the mixture with ethyl acetate (3×20 ml)
- washby washing of the
- extractionextract with 2M HCl (x2), 2M NaOH and evaporation of volatiles in vacuo