反应详情

温度

0 °C

Stir under N2 at 0° C. a suspension of NaH (29 mg, 0.72 mmol of 60% oil dispersion) in 1-methyl-2-pyrrolidinone (15 mL), and slowly add N,N-diethylethanolamine(0.095 mL, 0.72 mmol). Stir for 10 min and then add dropwise 3-(pyridin-4-ylamino)-1H-indole-2-carboxylic acid pentafluorophenyl ester (100 mg, 0.24 mmol). Allow the reaction to reach ambient temperature and stir overnight. Quench into water and extract with ethyl acetate. Wash the extract with water, brine, dry (MgSO4), filter and concentrate under vacuum to obtain crude product. Chromatograph on silica gel (10 g, Sepack cartridge) and use 1:1 methanol/ethyl acetate as eluent. Combine like fractions and concentrate under vacuum to obtain 26.3 mg (31%) of the titled compound: MS 353 (M+H).

1. stirringStir for 10 min
2. customthe reaction
3. customto reach ambient temperature
4. stirringstir overnight
5. customQuench into water
6. extractionextract with ethyl acetate
7. washWash the
8. extractionextract with water, brine
9. dry with materialdry (MgSO4)
10. filtrationfilter
11. concentrationconcentrate under vacuum
12. customto obtain crude product
13. concentrationCombine like fractions and concentrate under vacuum