Pyridine → 1-Phthalimido-4-p-toluenesulfonyl-7,7-difluoro-8-methanesulfonyloxy-4-aza-octane

To a solution of 1-phthalimido-4-p-toluenesulfonyl-7,7-difluoro-8-hydroxy-4-aza-octane (56.0 g, 120 mmoles) and dry pyridine (50 mL) in dry dichloromethane (400 mL), a solution of methanesulfonylchloride (14.4 g, 1.05 equivalents) in dichloromethane is added slowly at room temperature. After stirring overnight at room temperature, the mixture is washed with 1N HCl (500 mL), 10% aqueous NaHSO3 (250 mL), and water (250 mL). Drying (Na2SO4) and evaporation of the solvent yields an oil which solidifies under oil pump vacuum. Digestion with an acetone/cyclohexane mixture gives colorless crystals of 1-phthalimido-4-p-toluenesulfonyl-7,7-difluoro-8-methanesulfonyloxy-4-aza-octane.

1. washthe mixture is washed with 1N HCl (500 mL), 10% aqueous NaHSO3 (250 mL), and water (250 mL)
2. customDrying
3. custom(Na2SO4) and evaporation of the solvent
4. customyields an oil which

ORDレコード

ord-292c7899093f4b8e918ff45b63924d8d

出典データセット

uspto-grants-1989_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04851448