2-chloroprop-2-enyl 2-fluoro-2-oxoacetate

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Under dry N2 in flame dried glass apparatus, cesium fluoride (167 g, 1.1 mol) was placed in a 1 liter single neck flask and placed under high vacuum and gently heated with a flame until the solid became free flowing, then cooled to room temperature. Acetonitrile, distilled from CaH2 (183 ml) was added and the mixture cooled to -20° C. internal temperature. 2-Chloroallyl oxalochloride (183 g, 1.0 mol) was added dropwise over a 30 minute period and the mixture slowly warmed to room temperature, stirred at that temperature for 16 hours, and byproduct cesium chloride recovered by filtration with acetonitrile wash. The filtrate and wash were combined and stripped, and the residue distilled at reduced temperature to yield 129 g (77%) of the desired product, b.p. 62°-64° C./22 mm. Under dry N2 in flame was placed in a 1 liter single neck flask gently heated with a flame until the solid Acetonitrile, distilled from CaH2 (183 ml) was added the mixture cooled to -20° C. internal temperature the mixture slowly warmed to room temperature byproduct cesium chloride recovered by filtration with acetonitrile wash The filtrate and wash the residue distilled at reduced temperature

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Under dry N2 in flame dried glass apparatus, cesium fluoride (167 g, 1.1 mol) was placed in a 1 liter single neck flask and placed under high vacuum and gently heated with a flame until the solid became free flowing, then cooled to room temperature. Acetonitrile, distilled from CaH2 (183 ml) was added and the mixture cooled to -20° C. internal temperature. 2-Chloroallyl oxalochloride (183 g, 1.0 mol) was added dropwise over a 30 minute period and the mixture slowly warmed to room temperature, stirred at that temperature for 16 hours, and byproduct cesium chloride recovered by filtration with acetonitrile wash. The filtrate and wash were combined and stripped, and the residue distilled at reduced temperature to yield 129 g (77%) of the desired product, b.p. 62°-64° C./22 mm. Under dry N2 in flame was placed in a 1 liter single neck flask gently heated with a flame until the solid Acetonitrile, distilled from CaH2 (183 ml) was added the mixture cooled to -20° C. internal temperature the mixture slowly warmed to room temperature byproduct cesium chloride recovered by filtration with acetonitrile wash The filtrate and wash the residue distilled at reduced temperature

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Under dry N2 in flame dried glass apparatus, cesium fluoride (167 g, 1.1 mol) was placed in a 1 liter single neck flask and placed under high vacuum and gently heated with a flame until the solid became free flowing, then cooled to room temperature. Acetonitrile, distilled from CaH2 (183 ml) was added and the mixture cooled to -20° C. internal temperature. 2-Chloroallyl oxalochloride (183 g, 1.0 mol) was added dropwise over a 30 minute period and the mixture slowly warmed to room temperature, stirred at that temperature for 16 hours, and byproduct cesium chloride recovered by filtration with acetonitrile wash. The filtrate and wash were combined and stripped, and the residue distilled at reduced temperature to yield 129 g (77%) of the desired product, b.p. 62°-64° C./22 mm. Under dry N2 in flame was placed in a 1 liter single neck flask gently heated with a flame until the solid Acetonitrile, distilled from CaH2 (183 ml) was added the mixture cooled to -20° C. internal temperature the mixture slowly warmed to room temperature byproduct cesium chloride recovered by filtration with acetonitrile wash The filtrate and wash the residue distilled at reduced temperature

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Under dry N2 in flame dried glass apparatus, cesium fluoride (167 g, 1.1 mol) was placed in a 1 liter single neck flask and placed under high vacuum and gently heated with a flame until the solid became free flowing, then cooled to room temperature. Acetonitrile, distilled from CaH2 (183 ml) was added and the mixture cooled to -20° C. internal temperature. 2-Chloroallyl oxalochloride (183 g, 1.0 mol) was added dropwise over a 30 minute period and the mixture slowly warmed to room temperature, stirred at that temperature for 16 hours, and byproduct cesium chloride recovered by filtration with acetonitrile wash. The filtrate and wash were combined and stripped, and the residue distilled at reduced temperature to yield 129 g (77%) of the desired product, b.p. 62°-64° C./22 mm. Under dry N2 in flame was placed in a 1 liter single neck flask gently heated with a flame until the solid Acetonitrile, distilled from CaH2 (183 ml) was added the mixture cooled to -20° C. internal temperature the mixture slowly warmed to room temperature byproduct cesium chloride recovered by filtration with acetonitrile wash The filtrate and wash the residue distilled at reduced temperature

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Under dry N2 in flame dried glass apparatus, cesium fluoride (167 g, 1.1 mol) was placed in a 1 liter single neck flask and placed under high vacuum and gently heated with a flame until the solid became free flowing, then cooled to room temperature. Acetonitrile, distilled from CaH2 (183 ml) was added and the mixture cooled to -20° C. internal temperature. 2-Chloroallyl oxalochloride (183 g, 1.0 mol) was added dropwise over a 30 minute period and the mixture slowly warmed to room temperature, stirred at that temperature for 16 hours, and byproduct cesium chloride recovered by filtration with acetonitrile wash. The filtrate and wash were combined and stripped, and the residue distilled at reduced temperature to yield 129 g (77%) of the desired product, b.p. 62°-64° C./22 mm. Under dry N2 in flame was placed in a 1 liter single neck flask gently heated with a flame until the solid Acetonitrile, distilled from CaH2 (183 ml) was added the mixture cooled to -20° C. internal temperature the mixture slowly warmed to room temperature byproduct cesium chloride recovered by filtration with acetonitrile wash The filtrate and wash the residue distilled at reduced temperature

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Under dry N2 in flame dried glass apparatus, cesium fluoride (167 g, 1.1 mol) was placed in a 1 liter single neck flask and placed under high vacuum and gently heated with a flame until the solid became free flowing, then cooled to room temperature. Acetonitrile, distilled from CaH2 (183 ml) was added and the mixture cooled to -20° C. internal temperature. 2-Chloroallyl oxalochloride (183 g, 1.0 mol) was added dropwise over a 30 minute period and the mixture slowly warmed to room temperature, stirred at that temperature for 16 hours, and byproduct cesium chloride recovered by filtration with acetonitrile wash. The filtrate and wash were combined and stripped, and the residue distilled at reduced temperature to yield 129 g (77%) of the desired product, b.p. 62°-64° C./22 mm. Under dry N2 in flame was placed in a 1 liter single neck flask gently heated with a flame until the solid Acetonitrile, distilled from CaH2 (183 ml) was added the mixture cooled to -20° C. internal temperature the mixture slowly warmed to room temperature byproduct cesium chloride recovered by filtration with acetonitrile wash The filtrate and wash the residue distilled at reduced temperature