反应详情

温度

0 °C

To a stirred solution of 10-3 (3.38 g, 16.3 mmol) in CHCl3 (80 mL) was added saturated NaHCO3 (50 mL) and it was then chilled to 0° C. A solution of chloroacetyl chloride (1.94 mL, 24.4 mmol) in CHCl3 (30 mL) was added dropwise to the chilled biphase. Upon addition completion, the reaction was stirred at 0° C. for 1 h. The layers were separated and the aqueous layer was extracted twice with EtOAc. The combined organic layers were washed with brine, dried (Na2SO4) and concentrated to give 10-4 which was used without further purification in the next step.

1. additionUpon addition completion
2. customThe layers were separated
3. extractionthe aqueous layer was extracted twice with EtOAc
4. washThe combined organic layers were washed with brine
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated
7. customto give 10-4 which
8. customwas used without further purification in the next step