1,1,2,3,3-五甲基-2H-茚

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

实验步骤: To a solution of 11 g of 1,1,2,3,3-pentamethyl indane (0.058 mole) and 7 g of succinic anhydride (0.07 mole) in 100 cm3 of anhydrous 1,2-dichloroethane, stirred at 0° C., there are added, by small portions, 9.4 g of aluminum chloride in a manner such that the temperature remains lower than 30° C. The reaction mixture is stirred for 3 hours at ambient temperature and then poured into 250 cm3 of ice water. The organic phase is decanted and the aqueous phase is extracted twice with 1,2-dichloroethane. The organic phases are combined, washed with water and dried on magnesium sulfate. The solvent is evaporated under reduced pressure and the resulting product is crystallized in isopropyl ether. 7 g of 4-(1,1,2,3,3-pentamethyl-5-indanyl)-4-oxo butyric acid in the form of white crystals whose melting point is 161° C. are obtained. remains lower than 30° C The organic phase is decanted the aqueous phase is extracted twice with 1,2-dichloroethane washed with water dried on magnesium sulfate The solvent is evaporated under reduced pressure the resulting product is crystallized in isopropyl ether

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

实验步骤: prepared according to the disclosure of U.S. Pat. No. 4,902,840 issued on Feb. 20, 1990, the specification for which is incorporated herein by reference; 20% 1,1,2,3,3-pentamethylindane and 35% hexahydro-1,1,2,3,3-pentamethylindane is heated to 150° C. Hydrogen chloride gas evolves and is passed through a caustic soda scrubber. This solution is then washed with a 5% aqueous sodium hydroxide solution, dried over anhydrous magnesium sulfate and used without further purification in the next step, the carrying out of an oxo-reaction. prepared This solution is then washed with a 5% aqueous sodium hydroxide solution dried over anhydrous magnesium sulfate used without further purification in the next step the carrying out of an oxo-reaction

反应条件: temp:25.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Into a 500 ml reaction vessel equipped with stirrer, thermometer, reflux condenser, addition funnel and cooling bath is placed 50 grams of 1,1,2,3,3-pentamethyl indane having the structure: ##STR36## in admixture with 100 grams of acetic acid. While maintaining the reaction mass at 25° C., 40 grams of fuming nitric acid is added over a period of 0.5 hour. The reaction mass is then stirred for a period of 6 minutes. Over a period of 10 minutes while maintaining the reaction mass at 20°-22° C., 10 grams of concentrated sulfuric acid is added to the reaction mass. The reaction mass is then heated to a temperature in the range of 26°-30° C. with stirring and maintained at that temperature for a period of four hours. At the end of the four hour period, the reaction mass is added to water and a solid is formed which precipitates out. The resulting crystals are washed with two 500 ml portions of water. The crystals melt at 99.5° C. Into a 500 ml reaction vessel equipped with stirrer thermometer, reflux condenser, addition funnel cooling bath Over a period of 10 minutes while maintaining the reaction mass at 20°-22° C. The reaction mass is then heated to a temperature in the range of 26°-30° C. with stirring maintained at that temperature for a period of four hours a solid is formed which precipitates out The resulting crystals are washed with two 500 ml portions of water melt at 99.5° C.

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

实验步骤: To a solution of 11 g of 1,1,2,3,3-pentamethyl indane (0.058 mole) and 7 g of succinic anhydride (0.07 mole) in 100 cm3 of anhydrous 1,2-dichloroethane, stirred at 0° C, there are added, by small portions, 9.4 g of aluminum chloride in a manner such that the temperature remains lower than 30° C. The reaction mixture is stirred for 3 hours at ambient temperature and then poured into 250 cm3 of ice water. The organic phase is decanted and the aqueous phase is extracted twice with 1,2-dichloroethane. The organic phases are combined, washed with water and dried on magnesium sulfate. The solvent is evaporated under reduced pressure and the resulting product is crystallized in isopropyl ether. 7 g of 4-(1,1,2,3,3-pentamethyl-5-indanyl)-4-oxo butyric acid in the form of white crystals whose melting point is 161° C. are obtained. remains lower than 30° C The organic phase is decanted the aqueous phase is extracted twice with 1,2-dichloroethane washed with water dried on magnesium sulfate The solvent is evaporated under reduced pressure the resulting product is crystallized in isopropyl ether

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

实验步骤: To a mixture, stirred at ambient temperature in the absence of the humidity of the air, of 25 g of 1,1,2,3,3-pentamethyl indane and 13 cm3 of acetyl chloride, there are added, in small portions, 23 g of aluminum chloride in a manner such that the temperature does not exceed 40° C. Stirring is maintained for 2 hours after the end of the addition and the reaction mixture is left overnight. The next day, it is poured into 200 cm3 of ice water and then extracted three times with 150 cm3 of dichloromethane. The organic phases are combined, washed with sodium bicarbonate and then with water and dried on magnesium sulfate. The solvent is removed by evaporation under a vacuum and 31 g of 5-acetyl-1,1,2,3,3-pentamethyl indane in liquid form which is directly used for the following reactions are obtained. does not exceed 40° C is maintained for 2 hours after the end of the addition extracted three times with 150 cm3 of dichloromethane washed with sodium bicarbonate with water and dried on magnesium sulfate The solvent is removed by evaporation under a vacuum and 31 g of 5-acetyl-1,1,2,3,3-pentamethyl indane in liquid form which are obtained

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

实验步骤: To a solution of 11 g of 1,1,2,3,3-pentamethyl indane (0.058 mole) and 7 g of succinic anhydride (0.07 mole) in 100 cm3 of anhydrous 1,2-dichloroethane, stirred at 0° C., there are added, by small portions, 9.4 g of aluminum chloride in a manner such that the temperature remains lower than 30° C. The reaction mixture is stirred for 3 hours at ambient temperature and then poured into 250 cm3 of ice water. The organic phase is decanted and the aqueous phase is extracted twice with 1,2-dichloroethane. The organic phases are combined, washed with water and dried on magnesium sulfate. The solvent is evaporated under reduced pressure and the resulting product is crystallized in isopropyl ether. 7 g of 4-(1,1,2,3,3-pentamethyl-5-indanyl)-4-oxo butyric acid in the form of white crystals whose melting point is 161° C. are obtained. remains lower than 30° C The organic phase is decanted the aqueous phase is extracted twice with 1,2-dichloroethane washed with water dried on magnesium sulfate The solvent is evaporated under reduced pressure the resulting product is crystallized in isopropyl ether

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

实验步骤: prepared according to the disclosure of U.S. Pat. No. 4,902,840 issued on Feb. 20, 1990, the specification for which is incorporated herein by reference; 20% 1,1,2,3,3-pentamethylindane and 35% hexahydro-1,1,2,3,3-pentamethylindane is heated to 150° C. Hydrogen chloride gas evolves and is passed through a caustic soda scrubber. This solution is then washed with a 5% aqueous sodium hydroxide solution, dried over anhydrous magnesium sulfate and used without further purification in the next step, the carrying out of an oxo-reaction. prepared This solution is then washed with a 5% aqueous sodium hydroxide solution dried over anhydrous magnesium sulfate used without further purification in the next step the carrying out of an oxo-reaction