Water → 2-[4-(2-hydroxyethyl)piperazin-1-yl]-N-[2,4 bis(2,2,2-trifluoroethoxy)-6-methylpyridin-3-yl]acetamide

1-(2-Hydroxyethyl)piperazine (1.95 g, 15.0 mmol) and 2-bromo-N-[2,4-bis(2,2,2-trifluoroethoxy)-6-methylpyridin-3-yl]acetamide (5.00 g, 12.5 mmol) were dissolved in acetonitrile (30 mL). Potassium carbonate (2.25 g, 16.3 mmol) was added to the solution, followed by stirring for 5 hours at room temperature. The reaction mixture was dilluted with water, followed by extraction with ethyl acetate. The organic layer was sequentially washed with water and saturated brine, followed by drying over sodium sulfate anhydrate and concentration under reduced pressure. The obtained residue was purified through silica gel column chromatography (eluent: ammonia-saturated methanol/chloroform=1/20), to thereby yield 5.40 g of N-[2,4-bis(2,2,2-trifluoroethoxy)-6-methylpyridin-3-yl]-2-[4-(2-hydroxyethyl)piperazin-1-yl]acetamide as colorless crystals (yield 91%).

1. extractionfollowed by extraction with ethyl acetate
2. washThe organic layer was sequentially washed with water and saturated brine
3. dry with materialby drying over sodium sulfate anhydrate and concentration under reduced pressure
4. customThe obtained residue was purified through silica gel column chromatography (eluent: ammonia-saturated methanol/chloroform=1/20)

ORD 기록

ord-671738e2cbb344368e3704131c876b7b

출처 데이터셋

uspto-grants-2008_12

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US07459552B2