反应详情

温度

0 °C

2-Methoxyacetyl chloride (0.074 mL, 0.76 mmol) was added to a solution of 4-chloro-5-(trifluoromethyl)-1H-pyrrolo[2,3-b]pyridin-3-amine (120 mg, 0.51 mmol, Example 12, Steps A-G) in pyridine (5 mL) at 0° C. The reaction was stirred at 0° C. for 10 minutes, and the pyridine was removed in vacuo. The residue obtained was dissolved in THF (5 mL), treated with 2N LiOH (3 mL) and stirred for 20 minutes. THF was then removed under reduced pressure, and the aqueous slurry obtained was extracted with water (20 mL) and ethyl acetate (50 mL). The organic layer was separated, washed with brine, dried (Na2SO4) and concentrated in vacuo to provide N-(4-chloro-5-(trifluoromethyl)-1H-pyrrolo[2,3-b]pyridin-3-yl)-2-methoxyacetamide (154 mg, 98% yield) as a solid.

1. customthe pyridine was removed in vacuo
2. customThe residue obtained
3. stirringstirred for 20 minutes
4. customTHF was then removed under reduced pressure
5. customthe aqueous slurry obtained
6. extractionwas extracted with water (20 mL) and ethyl acetate (50 mL)
7. customThe organic layer was separated
8. washwashed with brine
9. dry with materialdried (Na2SO4)
10. concentrationconcentrated in vacuo