反应详情

温度

20 °C

Triethylamine (0.82 ml, 1.6 eq) and 3-bromobenzylbromide (0.97 g, 1 eq) are added successively to a solution of methyl 1-{3-[methyl(2-pyridin-2-ylethyl)amino]propyl}-2-thioxo-2,3-dihydro-1H-benzimidazole-5-carboxylate (1.5 g) in tetrahydrofuran (30 ml). The mixture is stirred for 15 hours at approximately 20° C. then concentrated under reduced pressure at 40° C. The residue obtained is diluted in ethyl acetate and water. After decanting and extracting, the organic phases are washed with salt water, dried over sodium sulphate and concentrated under reduced pressure at 40° C. Purification by flash chromatography on silica gel (eluent: dichloromethane/methanol 95/5 to 90/10) produces the expected compound in the form of a colourless oil (1.5 g; 70% yield).

1. concentrationthen concentrated under reduced pressure at 40° C
2. customThe residue obtained
3. customAfter decanting
4. extractionextracting
5. washthe organic phases are washed with salt water
6. dry with materialdried over sodium sulphate
7. concentrationconcentrated under reduced pressure at 40° C
8. customPurification by flash chromatography on silica gel (eluent: dichloromethane/methanol 95/5 to 90/10)