反应详情

温度

0 °C

1,4-Dioxaspiro[4.5]decan-8-ol (0.25 g, 1.58 mmol) and 2-[2-chloro-6-(trifluoromethyl)pyridin-4-yl]propan-2-ol (0.2 g, 0.835 mmol) were dissolved in tetrahydrofuran (2 mL) and cooled to 0° C. and a 60% mixture of sodium hydride (70.0 mg, 1.75 mmol) in mineral oil was added and the reaction was stirred for 30 minutes at 0° C. and at 25° C. for 60 hours at which time TLC analysis indicated the presence of some product. The reaction was quenched with water, and was extracted with ethyl acetate and the organic extracts were washed with water, saturated NaCl, dried (MgSO4), and evaporated in vacuo. The residue was purified by LC (pH 2) to give the product. MS (ES): 362 (M+1).

1. customThe reaction was quenched with water
2. extractionwas extracted with ethyl acetate
3. washthe organic extracts were washed with water, saturated NaCl
4. dry with materialdried (MgSO4)
5. customevaporated in vacuo
6. customThe residue was purified by LC (pH 2)
7. customto give the product