Chloroacetyl chloride → HCID 67597500, compound

Participants

Reaction Conditions

Reaction Steps

A solution of the product from Step C (0.590 g, 1.98 mmol) in ethyl acetate (30 mL) was vigorously stirred at 0° C. with saturated sodium bicarbonate (30 mL). Chloroacetyl chloride (0.315 mL, 3.96 mmol) was added, and the reaction stirred at 0° C. for 1 h. The layers were separated, and the ethyl acetate phase was washed with saturated brine, and dried over magnesium sulfate. The crude product was dissolved in DMF (15 mL) and cooled to 0° C. under nitrogen. Cesium carbonate (1.67 g, 5.12 mmol) was added and the reaction stirred 1 h at 0° C., then at room temperature overnight. The reaction was quenched with amminium chloride, and partitioned between ethyl acetate and water. The organic phase was washed with water, saturated brine, and dried over magnesium sulfate. The title compound was obtained as a colorless oil.

Provenance & Evidence