益康唑杂质11

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

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

实验步骤: A mixture of 8.4 g (89.2 mmol) 2-aminopyridine and 20.1 g (89.9 mmol) of 2,2′,4′-trichloroacetophenone in 300 ml of ethanol was heated at reflux with stirring for 14 h. At this point, another 5.0 g (22.4 mmol) of 2,2′, 4′-trichloroacetophenone was added and the reaction mixture heated an additional 6 h. Ethyl acetate (400 ml) and excess saturated aqueous sodium bicarbonate were slowly added. After thorough mixing, the ethyl acetate layer was separated and washed with two fold excess water, saturated brine, and dried over magnesium sulfate. Evaporating the solvent in vacuo to almost dryness gave a wet solid residue to which n-butyl chloride was added. This solid was filtered and washed thoroughly with n-butyl chloride before drying. A yield of 9.0 g of the title compound was obtained (m.p. 173-175° C.) as a technical material which was not purified further but used directly in the next step. was heated at reflux the reaction mixture heated an additional 6 h After thorough mixing, the ethyl acetate layer was separated washed with two fold excess water, saturated brine dried over magnesium sulfate Evaporating the solvent in vacuo to almost dryness gave a wet solid residue to which n-butyl chloride was added This solid was filtered washed thoroughly with n-butyl chloride before drying

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

实验步骤: A mixture of 8.4 g (89.2 mmol) 2-aminopyridine and 20.1 g (89.9 mmol) of 2,2′,4′-trichloroacetophenone in 300 ml of ethanol was heated at reflux with stirring for 14 h. At this point, another 5.0 g (22.4 mmol) of 2,2′, 4′-trichloroacetophenone was added and the reaction mixture heated an additional 6 h. Ethyl acetate (400 ml) and excess saturated aqueous sodium bicarbonate were slowly added. After thorough mixing, the ethyl acetate layer was separated and washed with two fold excess water, saturated brine, and dried over magnesium sulfate. Evaporating the solvent in vacuo to almost dryness gave a wet solid residue to which n-butyl chloride was added. This solid was filtered and washed thoroughly with n-butyl chloride before drying. A yield of 9.0 g of the title compound was obtained (m.p. 173-175° C.) as a technical material which was not purified further but used directly in the next step. was heated at reflux the reaction mixture heated an additional 6 h After thorough mixing, the ethyl acetate layer was separated washed with two fold excess water, saturated brine dried over magnesium sulfate Evaporating the solvent in vacuo to almost dryness gave a wet solid residue to which n-butyl chloride was added This solid was filtered washed thoroughly with n-butyl chloride before drying

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

实验步骤: Cultivation, reaction and purification were carried out in the same way as described in Example 9 except that 2-chloro-1-(2', 4'-dichlorophenyl) ethanon, 2-chloro-1-(3', 4'-dichlorophenyl) ethanone, 2-chloro-1-(2', 5'-dichlorophenyl) ethanone were used as substrate, and (-)-2-chloro-1-(2', 4'-dichlorophenyl) ethanol, (-)-2-chloro-1-(3', 4'-dichlorophenyl) ethanol, (-)-2-chloro-1-(2', 5'-dichlorophenyl) ethanol was obtained. The yield, specific rotation and optical purity determined by high-performance liquid chromatography were shown in Table 6. Cultivation, reaction and purification

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

实验步骤: Cultivation, reaction and purification were carried out in the same way as described in Example 9 except that 2-chloro-1-(2', 4'-dichlorophenyl) ethanon, 2-chloro-1-(3', 4'-dichlorophenyl) ethanone, 2-chloro-1-(2', 5'-dichlorophenyl) ethanone were used as substrate, and (-)-2-chloro-1-(2', 4'-dichlorophenyl) ethanol, (-)-2-chloro-1-(3', 4'-dichlorophenyl) ethanol, (-)-2-chloro-1-(2', 5'-dichlorophenyl) ethanol was obtained. The yield, specific rotation and optical purity determined by high-performance liquid chromatography were shown in Table 6. Cultivation, reaction and purification

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

实验步骤: 3.78 g (0.02 mole) of 4-n-heptyl-thiosemicarbazide and 4.67 g (0.02 mole) of 2,4-dichlorophenacyl chloride are reacted analogously to Example 1. After recrystallization from methanol/methyl acetate, 5.2 g of 5-(2,4-dichlorophenyl)-N-heptyl-6H-1,3,4-thiadiazin-2-amine monohydrochloride are produced. m.p. 175°-177° C. After recrystallization from methanol/methyl acetate, 5.2 g of 5-(2,4-dichlorophenyl)-N-heptyl-6H-1,3,4-thiadiazin-2-amine monohydrochloride are produced