Hydrochloric Acid → HCID 10601101, compound

Participants

Reaction Steps

3.50 g (6.80mmol) of 7-azido-6,8-difluoro-2-(3-fluoro-4-pivaloylaminophenyl)-5-pivaloylamino-4H-1-benzopyran-4-one obtained in Example 93 (1) was suspended in 120 mL of tetrahydrofuran, 1.96 g (7.48 mmol) of triphenylphosphine was added and the mixture was stirred at room temperature for 2 hours. To this was added 50 mL of 1N hydrochloric acid and the mixture was further stirred for 10 hours. The mixture was adjusted to pH 9 by addition of a 10N aqueous solution of sodium hydroxide thereto, and the precipitated crystals were collected by filtration and purified by silica gel column chromatography (chloroform-chloroform:methanol=40:l) to give 2.83 g of 7-amino-6,8-difluoro-2-(3-fluoro-4-pivaloylaminophenyl)-5-pivaloylamino-4H-1-benzopyran-4-one (yield: 85%).

Provenance & Evidence