反应详情

To trans-1-Hydroxy-cyclopropanecarboxylic acid {4-[2-(4-benzo[1,3]dioxol-4-yl-piperazin-1-yl)-ethyl]-cyclohexyl}-amide (20 mg, 48.1 μmol, Eq: 1.00) in THF (500 μl) was added NaH (3.37 mg, 84.2 μmol, Eq: 1.75) and methyl iodide (17.1 mg, 7.52 μl, 120 μmol, Eq: 2.5). After 2 hours the reaction mixture was diluted with water (300 ul). The crude reaction mixture was concentrated in vacuo. The residue was suspended with 5 mL sat NaHCO3 and extracted with dichloromethane (2×10 mL). The organic layers were dried over MgSO4 and concentrated in vacuo. The crude material was purified by flash chromatography (silica gel, 10 g, 0% to 15% MeOH in dichloromethane) to yield the title compound as an off-white solid (12.1 mg, 58.5%), MS (ISP) m/z=430.2 [(M+H)+].

1. customThe crude reaction mixture
2. concentrationwas concentrated in vacuo
3. extractionextracted with dichloromethane (2×10 mL)
4. dry with materialThe organic layers were dried over MgSO4
5. concentrationconcentrated in vacuo
6. customThe crude material was purified by flash chromatography (silica gel, 10 g, 0% to 15% MeOH in dichloromethane)