Propylene Glycol → HCID 46853062, compound

Participants

Reaction Steps

To a solution of step 3 intermediate (0.165 g, 0.78 mmol) in 3 mL of dry THF and pyridine (0.37 mL, 47 mmol) maintained at 0° C., oxalyl chloride was added with stirring. After 30 minutes propylene glycol (0.46 mL, 63 mmol) was added to the above reaction mixture and reaction warmed to room temperature. Reaction mixture was concentrated after adding ethyl alcohol. The residue was partitioned between 1N HCl and tert-butyl ether. Aqueous layer was separated and basified with 4N NaOH and extracted with ethyl acetate. Ethyl acetate layer was separated, dried and concentrated. Crude material was carried to next step without further purification. m/z (M+1): 170.2.

Provenance & Evidence