反应详情

温度

0 °C

In step 2-2, triethylamine (8.15 mL, 58.6 mmol) in a single portion was added to a solution of 2-amino-2-(3-fluorophenyl)ethanol (7.57 g, 48.8 mmol) in THF cooled to 0° C. and chloroacetyl chloride (5.08 mL, 58.6 mmol) was added drop-wise. The mixture was cooled to 0° C. and stirred for 1 hour. The reaction mixture was quenched with water and the organic phase was washed with 0.5 N HCl, saturated NaHCO3, brine, and dried over MgSO4. The organic phase was concentrated and purified with flash chromatography (50% EtOAc/hexanes) to yield 2-chloro-N-(1-(3-fluorophenyl)-2-hydroxyethyl)acetamide (2-2) as a yellow solid.

1. temperatureThe mixture was cooled to 0° C.
2. customThe reaction mixture was quenched with water
3. washthe organic phase was washed with 0.5 N HCl, saturated NaHCO3, brine
4. dry with materialdried over MgSO4
5. concentrationThe organic phase was concentrated
6. custompurified with flash chromatography (50% EtOAc/hexanes)