反应详情

To a stirred suspension of N-[2-({(2S)-3-[4-(5-fluoro-2-oxo-2,3-dihydro-1H-benzimidazol-1-yl)-1-piperidinyl]-2-hydroxypropyl}oxy)-4-methoxyphenyl]acetamide (Example 32 iii)) (0.17 g, 0.36 mmol) in CH2Cl2 (5 ml) with some drops of DMF a solution of boron tribromide (BBr3) in dichloromethane (CH2Cl2) (1M, 1.08 mmol, 1.08 ml) was added dropwise under nitrogen. The stirring was continued overnight art room temperature. Then the reaction mixture was quenched with methanol, diluted with water and extracted with dichloromethane (CH2Cl2) (2×10 ml) and ethyl acetate (2×10 ml). The combined organic extracts were dried with sodium sulphate and concentrated in vacuo. The residue was purified by flash chromatography of silica gel (CH2Cl2/MeOH, 9:1) to give a colourless solid (89 mg, 0.16 mmol, 45%).

1. additionwas added dropwise under nitrogen
2. customart room temperature
3. customThen the reaction mixture was quenched with methanol
4. additiondiluted with water
5. extractionextracted with dichloromethane (CH2Cl2) (2×10 ml) and ethyl acetate (2×10 ml)
6. dry with materialThe combined organic extracts were dried with sodium sulphate
7. concentrationconcentrated in vacuo
8. customThe residue was purified by flash chromatography of silica gel (CH2Cl2/MeOH, 9:1)