N1C=CC=CC=1.Cl[C:8]([O:10][CH2:11][Cl:12])=[O:9].[CH3:13][C:14]([OH:17])([CH3:16])[CH3:15]>C(Cl)Cl>[C:8](=[O:9])([O:10][CH2:11][Cl:12])[O:17][C:14]([CH3:16])([CH3:15])[CH3:13]0.62 mL pyridine was added dropwise to a solution of 0.77 g chloromethyl chloroformate and 1.32 mL t-BuOH in 60 mL CH2Cl2 cooled in an ice bath under an Ar atmosphere. The reaction was stirred 2 hours at 0° C. then transferred to a separatory funnel. The reaction was washed twice with H2O, once with 10% CuSO4, once with brine and dried with MgSO4. Suction filtration and evaporation provided 0.55 g of desired product which was used without purification.
読み込み中…