1,2-苯二硫醇

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

实验步骤: 15 g of dimercaptobenzene were slowly added dropwise while cooling to 5.55 g of sodium hydride (50% in mineral oil) in 150 ml of dimethyl sulfoxide, whereby the internal temperature was held between 15° and 23° C. Subsequently, the reaction mixture was stirred at room temperature for 1 hour and cooled with ice/methanol. Thereafter, 50 g of 2,2-dimethylpropanediol ditosylate in solid form were added in one portion and the reaction mixture was heated to 80° C. for 3 hours. Thereafter, the reaction mixture was cooled, poured on to ice, extracted with ether, the extract was washed with water and dried. After evaporation of the solvent, there was obtained a yellow oil which was chromatographed on silica gel (petroleum ether/ethyl acetate 99:1). There were obtained 14 g of 3,4-dihydro-3,3-dimethyl-2H-1,5-benzodithiepine as a colorless oil. was held between 15° and 23° C the reaction mixture was heated to 80° C. for 3 hours Thereafter, the reaction mixture was cooled poured on to ice extracted with ether the extract was washed with water dried After evaporation of the solvent there was obtained a yellow oil which was chromatographed on silica gel (petroleum ether/ethyl acetate 99:1)

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

实验步骤: The reaction was performed as described in Example 1, step 4, starting from ({[4-(tert-butoxycarbonyl)phenyl]methyl}cyclopentadienyl)dichloro(pentamethylcyclopentadienyl)titanium; i.e. reaction of the alkylated titanocene dichloride with benzenedithiol.

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

实验步骤: 15 g of dimercaptobenzene were slowly added dropwise while cooling to 5.55 g of sodium hydride (50% in mineral oil) in 150 ml of dimethyl sulfoxide, whereby the internal temperature was held between 15° and 23° C. Subsequently, the reaction mixture was stirred at room temperature for 1 hour and cooled with ice/methanol. Thereafter, 50 g of 2,2-dimethylpropanediol ditosylate in solid form were added in one portion and the reaction mixture was heated to 80° C. for 3 hours. Thereafter, the reaction mixture was cooled, poured on to ice, extracted with ether, the extract was washed with water and dried. After evaporation of the solvent, there was obtained a yellow oil which was chromatographed on silica gel (petroleum ether/ethyl acetate 99:1). There were obtained 14 g of 3,4-dihydro-3,3-dimethyl-2H-1,5-benzodithiepine as a colorless oil. was held between 15° and 23° C the reaction mixture was heated to 80° C. for 3 hours Thereafter, the reaction mixture was cooled poured on to ice extracted with ether the extract was washed with water dried After evaporation of the solvent there was obtained a yellow oil which was chromatographed on silica gel (petroleum ether/ethyl acetate 99:1)

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

实验步骤: 15 g of dimercaptobenzene were slowly added dropwise while cooling to 5.55 g of sodium hydride (50% in mineral oil) in 150 ml of dimethyl sulfoxide, whereby the internal temperature was held between 15° and 23° C. Subsequently, the reaction mixture was stirred at room temperature for 1 hour and cooled with ice/methanol. Thereafter, 50 g of 2,2-dimethylpropanediol ditosylate in solid form were added in one portion and the reaction mixture was heated to 80° C. for 3 hours. Thereafter, the reaction mixture was cooled, poured on to ice, extracted with ether, the extract was washed with water and dried. After evaporation of the solvent, there was obtained a yellow oil which was chromatographed on silica gel (petroleum ether/ethyl acetate 99:1). There were obtained 14 g of 3,4-dihydro-3,3-dimethyl-2H-1,5-benzodithiepine as a colorless oil. was held between 15° and 23° C the reaction mixture was heated to 80° C. for 3 hours Thereafter, the reaction mixture was cooled poured on to ice extracted with ether the extract was washed with water dried After evaporation of the solvent there was obtained a yellow oil which was chromatographed on silica gel (petroleum ether/ethyl acetate 99:1)

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

实验步骤: 15 g of dimercaptobenzene were slowly added dropwise while cooling to 5.55 g of sodium hydride (50% in mineral oil) in 150 ml of dimethyl sulfoxide, whereby the internal temperature was held between 15° and 23° C. Subsequently, the reaction mixture was stirred at room temperature for 1 hour and cooled with ice/methanol. Thereafter, 50 g of 2,2-dimethylpropanediol ditosylate in solid form were added in one portion and the reaction mixture was heated to 80° C. for 3 hours. Thereafter, the reaction mixture was cooled, poured on to ice, extracted with ether, the extract was washed with water and dried. After evaporation of the solvent, there was obtained a yellow oil which was chromatographed on silica gel (petroleum ether/ethyl acetate 99:1). There were obtained 14 g of 3,4-dihydro-3,3-dimethyl-2H-1,5-benzodithiepine as a colorless oil. was held between 15° and 23° C the reaction mixture was heated to 80° C. for 3 hours Thereafter, the reaction mixture was cooled poured on to ice extracted with ether the extract was washed with water dried After evaporation of the solvent there was obtained a yellow oil which was chromatographed on silica gel (petroleum ether/ethyl acetate 99:1)

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

实验步骤: 15 g of dimercaptobenzene were slowly added dropwise while cooling to 5.55 g of sodium hydride (50% in mineral oil) in 150 ml of dimethyl sulfoxide, whereby the internal temperature was held between 15° and 23° C. Subsequently, the reaction mixture was stirred at room temperature for 1 hour and cooled with ice/methanol. Thereafter, 50 g of 2,2-dimethylpropanediol ditosylate in solid form were added in one portion and the reaction mixture was heated to 80° C. for 3 hours. Thereafter, the reaction mixture was cooled, poured on to ice, extracted with ether, the extract was washed with water and dried. After evaporation of the solvent, there was obtained a yellow oil which was chromatographed on silica gel (petroleum ether/ethyl acetate 99:1). There were obtained 14 g of 3,4-dihydro-3,3-dimethyl-2H-1,5-benzodithiepine as a colorless oil. was held between 15° and 23° C the reaction mixture was heated to 80° C. for 3 hours Thereafter, the reaction mixture was cooled poured on to ice extracted with ether the extract was washed with water dried After evaporation of the solvent there was obtained a yellow oil which was chromatographed on silica gel (petroleum ether/ethyl acetate 99:1)

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

实验步骤: 15 g of dimercaptobenzene were slowly added dropwise while cooling to 5.55 g of sodium hydride (50% in mineral oil) in 150 ml of dimethyl sulfoxide, whereby the internal temperature was held between 15° and 23° C. Subsequently, the reaction mixture was stirred at room temperature for 1 hour and cooled with ice/methanol. Thereafter, 50 g of 2,2-dimethylpropanediol ditosylate in solid form were added in one portion and the reaction mixture was heated to 80° C. for 3 hours. Thereafter, the reaction mixture was cooled, poured on to ice, extracted with ether, the extract was washed with water and dried. After evaporation of the solvent, there was obtained a yellow oil which was chromatographed on silica gel (petroleum ether/ethyl acetate 99:1). There were obtained 14 g of 3,4-dihydro-3,3-dimethyl-2H-1,5-benzodithiepine as a colorless oil. was held between 15° and 23° C the reaction mixture was heated to 80° C. for 3 hours Thereafter, the reaction mixture was cooled poured on to ice extracted with ether the extract was washed with water dried After evaporation of the solvent there was obtained a yellow oil which was chromatographed on silica gel (petroleum ether/ethyl acetate 99:1)

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

实验步骤: 15 g of dimercaptobenzene were slowly added dropwise while cooling to 5.55 g of sodium hydride (50% in mineral oil) in 150 ml of dimethyl sulfoxide, whereby the internal temperature was held between 15° and 23° C. Subsequently, the reaction mixture was stirred at room temperature for 1 hour and cooled with ice/methanol. Thereafter, 50 g of 2,2-dimethylpropanediol ditosylate in solid form were added in one portion and the reaction mixture was heated to 80° C. for 3 hours. Thereafter, the reaction mixture was cooled, poured on to ice, extracted with ether, the extract was washed with water and dried. After evaporation of the solvent, there was obtained a yellow oil which was chromatographed on silica gel (petroleum ether/ethyl acetate 99:1). There were obtained 14 g of 3,4-dihydro-3,3-dimethyl-2H-1,5-benzodithiepine as a colorless oil. was held between 15° and 23° C the reaction mixture was heated to 80° C. for 3 hours Thereafter, the reaction mixture was cooled poured on to ice extracted with ether the extract was washed with water dried After evaporation of the solvent there was obtained a yellow oil which was chromatographed on silica gel (petroleum ether/ethyl acetate 99:1)

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

实验步骤: 15 g of dimercaptobenzene were slowly added dropwise while cooling to 5.55 g of sodium hydride (50% in mineral oil) in 150 ml of dimethyl sulfoxide, whereby the internal temperature was held between 15° and 23° C. Subsequently, the reaction mixture was stirred at room temperature for 1 hour and cooled with ice/methanol. Thereafter, 50 g of 2,2-dimethylpropanediol ditosylate in solid form were added in one portion and the reaction mixture was heated to 80° C. for 3 hours. Thereafter, the reaction mixture was cooled, poured on to ice, extracted with ether, the extract was washed with water and dried. After evaporation of the solvent, there was obtained a yellow oil which was chromatographed on silica gel (petroleum ether/ethyl acetate 99:1). There were obtained 14 g of 3,4-dihydro-3,3-dimethyl-2H-1,5-benzodithiepine as a colorless oil. was held between 15° and 23° C the reaction mixture was heated to 80° C. for 3 hours Thereafter, the reaction mixture was cooled poured on to ice extracted with ether the extract was washed with water dried After evaporation of the solvent there was obtained a yellow oil which was chromatographed on silica gel (petroleum ether/ethyl acetate 99:1)

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

实验步骤: To a solution of methyl propiolate (0.75 mL) in THF (10 mL) were added a solution of benzene-1,2-dithiol (1.2 g) in THF (10 mL) and tert-butoxy potassium (catalytic amount) under ice-cooling, and the mixture was stirred at the same temperature for 3 hours and then at room temperature for 3 hours. The reaction mixture was concentrated under reduced pressure. To the residue was added methanol (5 mL) at room temperature, and then an aqueous solution (10 mL) of sodium hydroxide (0.45 g). The mixture was stirred at 80° C. for 2 hours. To the reaction mixture was added ion-exchanged water (20 mL), which was washed with ethyl acetate. The aqueous layer was adjusted to pH 2 by addition of 1N hydrochloric acid, and then extracted with ethyl acetate (70 mL) twice. The organic layers were combined, washed with water and then a saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure to obtain 2-(benzo[1,3]dithiol-2-yl)acetic acid (1.35 g) as a yellow crystal. cooling at room temperature for 3 hours The reaction mixture was concentrated under reduced pressure To the residue was added methanol (5 mL) at room temperature The mixture was stirred at 80° C. for 2 hours To the reaction mixture was added ion-exchanged water (20 mL), which was washed with ethyl acetate The aqueous layer was adjusted to pH 2 by addition of 1N hydrochloric acid extracted with ethyl acetate (70 mL) twice washed with water a saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate concentrated under reduced pressure

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

实验步骤: 500 mgs (3.52 mmol) of 1,2-dimercaptobenzene and 610 mgs (3.00 mmol) of N-benzoyl-4-piperidone were stirred in CH2Cl2 while anhydrous HCl gas was introduced Na2SO4 (2 grams) was added and the mixture stirred 15 hours. The mixture was diluted with CH2Cl2 filtered and washed with H2O, and 10% NaOH. The organics were dried (Na2SO4) and concentrated to a solid (yield 740 mgs). was added filtered washed with H2O, and 10% NaOH The organics were dried (Na2SO4) concentrated to a solid (yield 740 mgs)

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

实验步骤: To a mixture of 3.0 grams (0.02 mole) dimercaptobenzene and 7.0 grams of potassium carbonate stirring in 50 ml of dimethylformamide, 3.5 grams of 2,5-dichloropyrimidine is added at 0° and the mixture stirred for 4 hours, before adding 5.0 grams of 2,5-dibromopyridine and heating at 80° for 4 additional hours. The mixture is added to excess H2O and extracted with ethyl ether. After washing the ether layer with H2O, saturated NaHCO3, brine, and drying (MgSO4), evaporating the solvent gives the crude product. is added at 0° heating at 80° for 4 additional hours extracted with ethyl ether After washing the ether layer with H2O, saturated NaHCO3, brine drying (MgSO4) evaporating the solvent