反应详情

A solution of 200 mg of amine from Example 62, 0.3 mL of DIPEA and 350 mg of 1-(RS)-(3,5-bis(trifluoromethyl)phenyl)ethyl bromide (prepared in Example 24) in 2 mL of acetonitrile was heated at 50° C. in a sealed vial for 40 h. The reaction was diluted with saturated sodium bicarbonate and extracted twice with methylene chloride. The organic layers were washed with a portion of brine, combined, dried over sodium sulfate and evaporated. The residue was purified by flash chromatography eluting with 10 to 15% ethyl acetate in hexanes to obtain 150 mg of title compound as a mixture of methyl isomers. Mass spec (NH3 /CI): 478 (M+1).

1. extractionextracted twice with methylene chloride
2. washThe organic layers were washed with a portion of brine
3. dry with materialdried over sodium sulfate
4. customevaporated
5. customThe residue was purified by flash chromatography
6. washeluting with 10 to 15% ethyl acetate in hexanes