反应详情

温度

-30 °C

Ms2O (18.65 mmol) was added at −30° C. to a solution of 2-[(4-chloro-phenyl)-hydroxy-methyl]-1-isopropyl-1H-pyrrole-3-carboxylic acid ethyl ester (Step E4) (9.32 mmol) and Et3N (46.6 mmol) in CH2Cl2 (60 mL) and stirred at −30° C. for 15 min. 3-Amino-5-chloro-1-methyl-1H-pyridin-2-one (Step L4) (11.19 mmol) was added and the mixture was stirred at −10° C. for 30 min. The mixture was diluted with H2O and extracted with CH2Cl2 (3×). The combined organic phases were washed successively with H2O and brine, dried (Na2SO4), filtered and concentrated. The residue was purified by flash chromatography to afford the title compound as a white solid. ESI-MS: tR=1.37 min, [M+]+462/464 (LC-MS 1).

1. stirringthe mixture was stirred at −10° C. for 30 min
2. extractionextracted with CH2Cl2 (3×)
3. washThe combined organic phases were washed successively with H2O and brine
4. dry with materialdried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated
7. customThe residue was purified by flash chromatography