Chloroacetyl chloride → HCID 69781315, compound

Participants

Reaction Steps

Chloroacetyl chloride (0.23 mL), 2.88 mmol) was added dropwise to a mixture of Intermediate 7 (0.82 g, 2.21 mmol) and Et3N (0.71 mL, 5.09 mmol) in CH2Cl2 (15 mL) at 0° C. under a nitrogen blanket. The resulting mixture was warmed to room temperature and stirred for about 0.5 hour. The reaction was quenched with 1 N HCl (2 mL), and diluted with CH2Cl2 (50 mL) and-water (10 mL). The layers were separated and the organic was washed with saturated NaCl and dried over anhydrous Na2SO4. Filtration and concentration in vacuo afforded Intermediate 8 (1.5 g), which was used without further purification. TLC Rf (10% EtOAc/CH2Cl2)=0.55; MS (API) m/z 448 (M+H), 472 (M+Na).

Provenance & Evidence