2-氯-9H-氧芴

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 2-chloro 9-fluorenone (18) (5 g, 23.3 mmoL), hydrazine monohydrate (6 mL, 120 mmoL, 5.2 eq) and acetic acid (1 mL) in ethanol (150 mL ) was refluxed for 2.5 h. The mixture was then evaporated to dryness to provide 5.3 g (100%) of product which was used without further purification: mp 139°-143° C.. was refluxed for 2.5 h The mixture was then evaporated to dryness

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A methanol free, 40% solution of Triton B in pyridine (8 mL) was added to a stirred, room temperature solution of commercially available (Alpha) 2-chlorofluorene (17) (42 g, 0.21 mmoL) in pyridine (257 mL) and oxygen was bubbled through the mixture at a moderate rate for 18 h. The majority of the pyridine was then removed on the rotary evaporator at reduced pressure and 5% aqueous hydrochloric acid (500 mL) was added to the residue. The solid was collected by filtration and washed with 5% aqueous hydrochloric acid and water. After drying, the solid was extracted repeatedly with hexane to remove some hexane insoluble impurities. Evaporation of the hexane left 42.7 g(95%) of 2-chloro-9-fluorenone: mp 110°-113° C. was bubbled through the mixture at a moderate rate for 18 h The majority of the pyridine was then removed on the rotary evaporator at reduced pressure and 5% aqueous hydrochloric acid (500 mL) was added to the residue The solid was collected by filtration washed with 5% aqueous hydrochloric acid and water After drying the solid was extracted repeatedly with hexane to remove some hexane insoluble impurities Evaporation of the hexane left 42.7 g(95%) of 2-chloro-9-fluorenone

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 2-chloro 9-fluorenone (18) (5 g, 23.3 mmoL), hydrazine monohydrate (6 mL, 120 mmoL, 5.2 eq) and acetic acid (1 mL) in ethanol (150 mL ) was refluxed for 2.5 h. The mixture was then evaporated to dryness to provide 5.3 g (100%) of product which was used without further purification: mp 139°-143° C.. was refluxed for 2.5 h The mixture was then evaporated to dryness

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A methanol free, 40% solution of Triton B in pyridine (8 mL) was added to a stirred, room temperature solution of commercially available (Alpha) 2-chlorofluorene (17) (42 g, 0.21 mmoL) in pyridine (257 mL) and oxygen was bubbled through the mixture at a moderate rate for 18 h. The majority of the pyridine was then removed on the rotary evaporator at reduced pressure and 5% aqueous hydrochloric acid (500 mL) was added to the residue. The solid was collected by filtration and washed with 5% aqueous hydrochloric acid and water. After drying, the solid was extracted repeatedly with hexane to remove some hexane insoluble impurities. Evaporation of the hexane left 42.7 g(95%) of 2-chloro-9-fluorenone: mp 110°-113° C. was bubbled through the mixture at a moderate rate for 18 h The majority of the pyridine was then removed on the rotary evaporator at reduced pressure and 5% aqueous hydrochloric acid (500 mL) was added to the residue The solid was collected by filtration washed with 5% aqueous hydrochloric acid and water After drying the solid was extracted repeatedly with hexane to remove some hexane insoluble impurities Evaporation of the hexane left 42.7 g(95%) of 2-chloro-9-fluorenone