Triethylamine → HCID 9895731, compound

Participants

Reaction Steps

To a solution of the compound obtained in Example 32 (1.39 g, 2.43 mmol) in dichioromethane (30 ml) are added 1,1′-carbonyldi-imidazole (0.79 g, 4.86 mmol) and triethylamine (0.68 ml, 4.86 mmol) with ice-cooling. Then the mixture is stirred at room temperature for 2 days. To this reaction mixture is added O-methylhydroxyamine hydrochloride(1.02 g, 12.2 mmol) and triethylamine (1.71 ml, 12.2 mmol) with ice-cooling. The reaction mixture is stirred at this temperature for 4 hours. To the residual mixture is added a mixture of chloroform (50 ml) and water (50 ml). The aqueous layer is extracted with chloroform (50 ml). The combined organic extract is dried over Na2SO4 and concentrated under reduced pressure to give the yellow residue, which is chromatographed on silica gel to afford white-brown crystalline solid. The solid is recrystallized from 2-propanol-ethyl acetate-isopropyl ether to afford pale yellow crystals (1.15 g, 73%).

Provenance & Evidence