HRID2422500
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
PROCEDURE
实验过程
To a solution of 1,1,1-trifluoro-4-(triisopropylsilyl)but-3-yn-2-one (3.00 g, 10.8 mmol) in CH2Cl2 (80 mL) at 0° C., was added a THF solution of allylmagnesium chloride (2.0 M, 8.08 mL, 16.2 mmol). After 1 h, a saturated solution of NH4Cl was added. The aqueous layer was extracted with CHCl3 (3×), and the combined organic layers were washed with H2O and brine, dried (Na2SO4) and concentrated under vacuum at 30° C. affording the title compound (3.63 g). 1H NMR (400 MHz, acetone-d6): 6.02 (m, 2H), 5.20-5.27 (m, 2H), 2.62 (m, 2H), 1.10 (m, 21H).
WORKUP
后处理
- extractionThe aqueous layer was extracted with CHCl3 (3×)
- washthe combined organic layers were washed with H2O and brine
- dry with materialdried (Na2SO4)
- concentrationconcentrated under vacuum at 30° C.