反应详情

温度

0 °C

(6-(3,5-dimethylisoxazol-4-yl)-2-ethoxy-1H-benzo[d]imidazol-4-yl)(pyridin-2-yl)methanone (50 mg, 0.14 mmol) was dissolved in dry THF (1.4 mL) under argon and cooled to 0° C. Cyclopentylmagnesium chloride (2.0 M, 0.14 mL, 0.28 mmol) was added dropwise and reaction was allowed to stir for 10 minutes then quenched with water. Reaction mixture was extracted three times with EtOAc and combined organic layers were washed once with water and concentrated. Residue was taken up in EtOH (1.5 mL) and 4.0M HCl/dioxane (0.75 mL) and heated to 65° C. for 2 hours. Reaction was concentrated and purified by reverse-phase HPLC to afford the desired product as a white powder.

1. customreaction
2. customthen quenched with water
3. customReaction mixture
4. extractionwas extracted three times with EtOAc
5. washwere washed once with water
6. concentrationconcentrated
7. temperature4.0M HCl/dioxane (0.75 mL) and heated to 65° C. for 2 hours
8. customReaction
9. concentrationwas concentrated
10. custompurified by reverse-phase HPLC