仲丁醇铝

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

实验步骤: To a flask containing 50.02 g of a mixture of heptane isomers was added 31.0 g (0.125 mol) of aluminium tris(sec-butoxide). To this was added with stirring, 48.37 g (0.376 mol) of ethylacetoacetate. After stirring the liquor was transferred to a rotary evaporator flask and the volatile sec-butanol and heptanes (78.66 g) were removed under vacuum leaving aluminium tris(ethylacetoacetate) (51.23 g, 0.124 mol). To this was added After stirring the liquor was transferred to a rotary evaporator flask the volatile sec-butanol and heptanes (78.66 g) were removed under vacuum

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

实验步骤: To a flask containing 50.02 g of a mixture of heptane isomers was added 31.0 g (0.125 mol) of aluminium tris(sec-butoxide). To this was added with stirring, 48.37 g (0.376 mol) of ethylacetoacetate. After stirring the liquor was transferred to a rotary evaporator flask and the volatile sec-butanol and heptanes (78.66 g) were removed under vacuum leaving aluminium tris(ethylacetoacetate) (51.23 g, 0.124 mol). To this was added After stirring the liquor was transferred to a rotary evaporator flask the volatile sec-butanol and heptanes (78.66 g) were removed under vacuum

反应条件: temp:155.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 1.0 grams of 3,10-dihexylpentacene-5,12-dione and 2.5 grams of aluminum tri(sec-butoxide) in 50 mL of mesitylene was heated to 155° C. for 2 days and cooled. The reaction mixture was filtered and the residue washed with concentrated HCl to give 2,9-dihexylpentacene. cooled The reaction mixture was filtered the residue washed with concentrated HCl

反应条件: temp:145.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 5.69 grams of aluminum tri(sec-butoxide) and 49.1 mLs of cyclohexanol was made. To this was added 2.21 grams 3,10-Dihexylpentacene-5,12-dione. The reaction mixture was heated to 145° C. for 24 hours. The mixture was cooled to room temperature and the solid isolated by centrifugation. The solid was stirred with 40 mLs of cyclohexanol and centrifuged two times. The solid was collected by filtration and washed with THF to give 2,9-dihexylpentacene. The mixture was cooled to room temperature the solid isolated by centrifugation The solid was collected by filtration washed with THF

反应条件: temp:145.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a 500 mL three necked round bottom flask with a thermometer, and a distillation head was added 32.76 grams of aluminum tri(sec-butoxide) and 200 mLs of cyclohexanol. To this was added 9 grams 3,10-Dimethylpentacene-5,12-dione. The reaction mixture was heated to 145° C. At 140° C., 8.7 grams of a distillate was collected. The reaction mixture was heated at 140° C. for 43 hours and cooled to room temperature. A solid was isolated by centrifugation. The supernate liquid was poured off and the solid was slurried with 140 mLs of 1N HCl and isolated on a Buchner funnel. The solid was slurried three times with 100 mLs each 1N HCl and the solvent was poured off each time. The solid was slurried three times with 100 mLs of acetone and isolated by filtration. The solid was slurried three times with 100 mLs of THF and isolated by filtration. The residue was air dried to give 2,9-dimethylpentacene. At 140° C., 8.7 grams of a distillate was collected The reaction mixture was heated at 140° C. for 43 hours cooled to room temperature A solid was isolated by centrifugation The supernate liquid was poured off isolated on a Buchner funnel the solvent was poured off each time isolated by filtration isolated by filtration dried

反应条件: temp:145.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 5.69 grams of aluminum tri(sec-butoxide) and 49.1 mLs of cyclohexanol was made. To this was added 2.21 grams 3,10-Dihexylpentacene-5,12-dione. The reaction mixture was heated to 145° C. for 24 hours. The mixture was cooled to room temperature and the solid isolated by centrifugation. The solid was stirred with 40 mLs of cyclohexanol and centrifuged two times. The solid was collected by filtration and washed with THF to give 2,9-dihexylpentacene. The mixture was cooled to room temperature the solid isolated by centrifugation The solid was collected by filtration washed with THF

反应条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a mixture of 0.5 grams of 2,9-difluoropentacene-5,7,12,14-tetrone and 20 mL of cyclohexanol in a flask was added 3.640 grams of aluminum tri(sec-butoxide). The mixture was heated at 100° C. for approximately 12 hours and a blue solid deposited on the sides of the flask. The reaction mixture was centrifuged and the blue solid residue was washed with cyclohexanol, centrifuged twice, and then washed with acetone and collected by filtration. This solid was washed with 50% concentrated HCl and the resulting mixture was centrifuged to give a blue solid. This solid was washed with THF and collected by centrifugation to give 2,9-difluoropentacene. the blue solid residue was washed with cyclohexanol washed with acetone collected by filtration This solid was washed with 50% concentrated HCl to give a blue solid This solid was washed with THF collected by centrifugation

反应条件: temp:145.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a mixture of 1.0 gram of pentacene-5,7,12,14-tetrone in 100 mL of cyclohexanol was added 7.3 grams of aluminum tri(sec-butoxide). The reaction mixture was heated to 145° C. for 66 hours. The reaction mixture was cooled to room temperature and placed in a centrifuge. A dark solid was separated and washed 3 times with cyclohexanol followed by centrifugation. The residue was washed with acetone, isolated on a filter flask, and air dried to give pentacene The reaction mixture was cooled to room temperature A dark solid was separated washed 3 times with cyclohexanol The residue was washed with acetone isolated on a filter flask air dried

反应条件: temp:145.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a mixture of 1.0 gram of pentacene-5,7,12,14-tetrone in 100 mL of cyclohexanol was added 7.3 grams of aluminum tri(sec-butoxide). The reaction mixture was heated to 145° C. for 66 hours. The reaction mixture was cooled to room temperature and placed in a centrifuge. A dark solid was separated and washed 3 times with cyclohexanol followed by centrifugation. The residue was washed with acetone, isolated on a filter flask, and air dried to give pentacene The reaction mixture was cooled to room temperature A dark solid was separated washed 3 times with cyclohexanol The residue was washed with acetone isolated on a filter flask air dried

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

实验步骤: Aluminum sec-butoxide was prepared in accordance with the process described in U.S. Pat. No. 4,242,271. A 75% mixed solution of this aluminum sec-butoxide in sec-butyl alcohol was hydrolyzed at 85° C. with a mixed solution of sec-butyl alcohol containing 30% of water to obtain an alumina slurry. After the alumina slurry was aged at 125° C. for 3 hours in an electromagnetically stirring autoclave, water was immediately added to the alumina slurry until a solids content was 20%, and the thus-treated alumina slurry was cooled. The pH of the alumina slurry was adjusted with a 3.8% aqueous solution of nitric acid to obtain Alumina Hydrate 6A. Alumina hydrate A obtained by drying colloidal sol of this alumina hydrate was determined by X-ray diffractometry and found to have a pseudoboehmite structure. At this time, the BET specific surface area was 175 m2/g, and the pore volume was 0.65 ml/g. Incidentally, the specific surface area and pore volume were determined by the following respective methods. to obtain an alumina slurry was immediately added to the alumina slurry until a solids content the thus-treated alumina slurry was cooled

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

实验步骤: Aluminum sec-butoxide was prepared in accordance with the process described in U.S. Pat. No. 4,242,271. A 75% mixed solution of this aluminum sec-butoxide in sec-butyl alcohol was hydrolyzed at 85° C. with a mixed solution of sec-butyl alcohol containing 30% of water to obtain an alumina slurry. After the alumina slurry Was aged at 125° C. for 3 hours in an electromagnetically stirring autoclave, water was immediately added to the alumina slurry until a solids content was 20%, and the thus-treated alumina slurry was cooled. The pH of the alumina slurry was adjusted with a 3.8% aqueous solution of nitric acid to obtain Alumina Hydrate 6A. Alumina hydrate A obtained by drying colloidal sol of this alumina hydrate was determined by X-ray diffractometry and found to have a pseudoboehmite structure. At this time, the BET specific surface area was 175 m2/g, and the pore volume was 0.65 ml/g. Incidentally, the specific surface area and pore volume were determined by the following respective methods. to obtain an alumina slurry was immediately added to the alumina slurry until a solids content the thus-treated alumina slurry was cooled

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

实验步骤: Aluminum sec-butoxide was prepared in accordance with the process described in U.S. Pat. No. 4,242,271. A 75% mixed solution of this aluminum sec-butoxide in sec-butyl alcohol was hydrolyzed at 85° C. with a mixed solution of sec-butyl alcohol containing 30% of water to obtain an alumina slurry. After the alumina slurry was aged at 125° C. for 3 hours in an electromagnetically stirring autoclave, water was immediately added to the alumina slurry until a solids content was 20%, and the thus-treated alumina slurry was cooled. The pH of the alumina slurry was adjusted with a 3.8% aqueous solution of nitric acid to obtain Alumina Hydrate 6A. Alumina hydrate A obtained by drying colloidal sol of this alumina hydrate was determined by X-ray diffractometry and found to have a pseudoboehmite structure. At this time, the BET specific surface area was 175 m2/g, and the pore volume was 0.65 ml/g. Incidentally, the specific surface area and pore volume were determined by the following respective methods. to obtain an alumina slurry was immediately added to the alumina slurry until a solids content the thus-treated alumina slurry was cooled