N-甲基-N'-(2,4-二甲基苯基)硫脲

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

实验步骤: 30.0 g of N-(2,4-dimethylphenyl)-N'-methyl-thiourea were stirred with 150 ml of 1,2-dimethoxy-ethane and 10 ml of triethylamine, and 36.0 g of a 30% strength aqueous solution of glyoxal was added. After stirring for a short time, the thiourea slowly dissolved, the reaction being exothermic. The temperature was allowed to rise to 50° C. and the solution was kept at this temperature for a further 1 hour. Thereafter, the solvent was distilled off in vacuo and the oily residue was stirred with water, with the addition of a little acetic acid. The reaction product, which solidified in the crystalline form, was filtered off, washed with water and dried. The yield was 37 g. For purification, the product could be recrystallised from isopropyl alcohol. was added to rise to 50° C. Thereafter, the solvent was distilled off in vacuo the oily residue was stirred with water, with the addition of a little acetic acid was filtered off washed with water dried For purification the product could be recrystallised from isopropyl alcohol

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

实验步骤: 3.41 g (0.01 mole) of 2-bromo-4'-chloro-3'-dimethylsulfamoyl-acetophenone are added to a solution of 1.83 g (0.01 mole) of 3-methyl-1-(2,4-dimethylphenyl)thiourea in 60 ml of glacial acetic acid and the mixture is stirred at room temperature for 20 minutes. It is then boiled for 20 minutes under a reflux condenser and allowed to cool, 60 ml of ethyl acetate or diisopropyl ether are added to the reaction mixture and the crystals are filtered off. Melting point 260°-264° C. (with decomposition). It is then boiled for 20 minutes under a reflux condenser to cool the crystals are filtered off

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

实验步骤: 30.0 g of N-(2,4-dimethylphenyl)-N'-methyl-thiourea were stirred with 150 ml of 1,2-dimethoxy-ethane and 10 ml of triethylamine, and 36.0 g of a 30% strength aqueous solution of glyoxal was added. After stirring for a short time, the thiourea slowly dissolved, the reaction being exothermic. The temperature was allowed to rise to 50° C. and the solution was kept at this temperature for a further 1 hour. Thereafter, the solvent was distilled off in vacuo and the oily residue was stirred with water, with the addition of a little acetic acid. The reaction product, which solidified in the crystalline form, was filtered off, washed with water and dried. The yield was 37 g. For purification, the product could be recrystallised from isopropyl alcohol. was added to rise to 50° C. Thereafter, the solvent was distilled off in vacuo the oily residue was stirred with water, with the addition of a little acetic acid was filtered off washed with water dried For purification the product could be recrystallised from isopropyl alcohol

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

实验步骤: 3.41 g (0.01 mole) of 2-bromo-4'-chloro-3'-dimethylsulfamoyl-acetophenone are added to a solution of 1.83 g (0.01 mole) of 3-methyl-1-(2,4-dimethylphenyl)thiourea in 60 ml of glacial acetic acid and the mixture is stirred at room temperature for 20 minutes. It is then boiled for 20 minutes under a reflux condenser and allowed to cool, 60 ml of ethyl acetate or diisopropyl ether are added to the reaction mixture and the crystals are filtered off. Melting point 260°-264° C. (with decomposition). It is then boiled for 20 minutes under a reflux condenser to cool the crystals are filtered off

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

实验步骤: 30.0 g of N-(2,4-dimethylphenyl)-N'-methyl-thiourea were stirred with 150 ml of 1,2-dimethoxy-ethane and 10 ml of triethylamine, and 36.0 g of a 30% strength aqueous solution of glyoxal was added. After stirring for a short time, the thiourea slowly dissolved, the reaction being exothermic. The temperature was allowed to rise to 50° C. and the solution was kept at this temperature for a further 1 hour. Thereafter, the solvent was distilled off in vacuo and the oily residue was stirred with water, with the addition of a little acetic acid. The reaction product, which solidified in the crystalline form, was filtered off, washed with water and dried. The yield was 37 g. For purification, the product could be recrystallised from isopropyl alcohol. was added to rise to 50° C. Thereafter, the solvent was distilled off in vacuo the oily residue was stirred with water, with the addition of a little acetic acid was filtered off washed with water dried For purification the product could be recrystallised from isopropyl alcohol

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

实验步骤: 19.4 g (0.1 mole) of N-2,4-xylyl-N'-methyl-thiourea and 15.2 g (0.1 mole) of chloroacetaldehyde-diethylacetal in 150 ml of 2N aqueous hydrochloric acid are refluxed for 1 hour. The clear light-yellow solution is subsequently cooled to room temperature; it is rendered slightly alkaline with 30% aqueous medium hydroxide solution, and extracted with ether. The ether extract is washed with water, dried with sodium sulphate and filtered, and the ether is then distilled off. The oily residue is distilled; b.p. 132°-134° C/0.3 Torr; yield: 20.2 g = 92% of theory. extracted with ether The ether extract is washed with water dried with sodium sulphate filtered the ether is then distilled off The oily residue is distilled

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

实验步骤: 3.41 g (0.01 mole) of 2-bromo-4'-chloro-3'-dimethylsulfamoyl-acetophenone are added to a solution of 1.83 g (0.01 mole) of 3-methyl-1-(2,4-dimethylphenyl)thiourea in 60 ml of glacial acetic acid and the mixture is stirred at room temperature for 20 minutes. It is then boiled for 20 minutes under a reflux condenser and allowed to cool, 60 ml of ethyl acetate or diisopropyl ether are added to the reaction mixture and the crystals are filtered off. Melting point 260°-264° C. (with decomposition). It is then boiled for 20 minutes under a reflux condenser to cool the crystals are filtered off