反应详情

To a solution of (2-{[(3,5-bis-trifluoromethyl-benzyl)-(2-methyl-2H-tetrazol-5-yl)-amino]-methyl}-4-trifluoromethyl-phenyl)-cyclopentyl-methanol (44,5 mg, 0.077 mmol) in methylene chloride (1.0 mL) at room temperature was added Dess-Martin periodinane reagent (35.7 mg, 0.084 mmol). The mixture was stirred at room temperature for 1.5 hours. Ether and 1N sodium hydroxide was added. The mixture was extracted with ethyl acetate. Combined organic layers were washed with brine, dried over sodium sulfate and concentrated in vacuo to yield a pale yellow oil (41.6 mg, 94%). 1H NMR (400 MHz, CDCl3) δ ppm 1.58-1.72 (m, 4H) 1.75-1.88 (m, 4H) 3.48-3.58 (m, 1H) 4.18 (s, 3H) 4.81 (s, 2H) 4.88 (s, 2H) 7.53 (s, 1H) 7.57 (d, J=8.30 Hz, 1H) 7.66 (s, 2H) 7.71 (d, 1H) 7.73 (s, 1H). MS (ES+) Calc: 579.2, Found: 580.4 (M+1).

1. extractionThe mixture was extracted with ethyl acetate
2. washCombined organic layers were washed with brine
3. dry with materialdried over sodium sulfate
4. concentrationconcentrated in vacuo