反应详情

To 0.53 g of 2-chloro-4-fluoro-5-nitrophenol XV-1 were added 3 ml of isopropanol, 3 ml of water and 0.72 g of sodium hydroxide, and the resultant mixture was heated at 50° to 60° C. while introducing chlorodifluoromethane gas for 4 hours. The mixture was stirred for 4 hours and during that period mixed twice with 0.50 g of sodium hydroxide at intervals of 1.5 hours. After cooling, the reaction mixture was neutralized with 2N hydrochloride acid and shaken with dichloromethane. The dichloromethane layer was dried and concentrated. The residue was chromatographed on a column of silica gel, eluting with n-hexane-ethylacetate (100:5 v/v). The eluate was concentrated to give 0.24 g of the titled compound XII-1.

1. temperatureAfter cooling
2. dry with materialThe dichloromethane layer was dried
3. concentrationconcentrated
4. customThe residue was chromatographed on a column of silica gel
5. washeluting with n-hexane-ethylacetate (100:5 v/v)
6. concentrationThe eluate was concentrated