反应详情

温度

80 °C

To a stirring RT slurry of NaH (0.10 g of a 60% by weight oil dispersion, 2.5 mmol) in DMF (2 mL) was added 5-amino-2-chlorophenol (0.20 g, 1.4 mmol). The mixture was stirred for 10 min before adding 1-(2-chloroethyl-pyrrolidine hydrochloride (0.17 g, 1.0 mmol). The reaction was heated at 80° C. for 15 h. The reaction was quenched with water, treated with 1N NaOH, and extracted twice with EtOAc. The combined organic layers were washed with brine, dried over Na2SO4, filtered, and concentrated in vacuo. The crude residue was purified by silica gel chromatography to yield title compound. MS: (MH+)=241.2; Calc'd 240.74 for C12H17ClN2O.

1. customThe reaction was quenched with water
2. additiontreated with 1N NaOH
3. extractionextracted twice with EtOAc
4. washThe combined organic layers were washed with brine
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customThe crude residue was purified by silica gel chromatography