反应 #4130082
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openreactiondata ↗doi:10.1039/C8SC04228D
反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-e49c56645a554acda01e832be1e74a91暂无可渲染的结构数据
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11 条反应 · 11 篇文献
反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-e49c56645a554acda01e832be1e74a91反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 6.8 of 2-bromo-4'-chloro-3'-dimethylsulfamoylacetophenone were reacted according to Example 23 with 3.3 g of 1,3-dipropylthiourea. After adding 200 ml of diethyl ether, 4-(4-chloro-3-dimethylsulfamoylphenyl)-3-propyl-2-propylimino-1,3-thiazolidine-4-ol-hydrobromide was separated as an oil. The solvent was decanted, the product was dissolved in 30 ml of water and extracted with 100 ml of ethyl acetate. After drying over sodium sulfate, the solvent was distilled off under reduced pressure, the amorphous residue was dissolved in 30 ml of ethanol and acidified with ethanolic hydrochloric acid. The solvent was distilled off, the residue was dissolved in 40 ml of water and the end product was obtained by lyophilization. Colorless amorphous solid body, decomposition beginning at 128° C, γ C=N1615 cm-1. was separated as an oil The solvent was decanted the product was dissolved in 30 ml of water extracted with 100 ml of ethyl acetate After drying over sodium sulfate the solvent was distilled off under reduced pressure the amorphous residue was dissolved in 30 ml of ethanol The solvent was distilled off the residue was dissolved in 40 ml of water the end product was obtained by lyophilization at 128° C
来源 ID: ord-88cfa64fe19a4ffcab3a66d6a399d3d7反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 6.8 of 2-bromo-4'-chloro-3'-dimethylsulfamoylacetophenone were reacted according to Example 23 with 3.3 g of 1,3-dipropylthiourea. After adding 200 ml of diethyl ether, 4-(4-chloro-3-dimethylsulfamoylphenyl)-3-propyl-2-propylimino-1,3-thiazolidine-4-ol-hydrobromide was separated as an oil. The solvent was decanted, the product was dissolved in 30 ml of water and extracted with 100 ml of ethyl acetate. After drying over sodium sulfate, the solvent was distilled off under reduced pressure, the amorphous residue was dissolved in 30 ml of ethanol and acidified with ethanolic hydrochloric acid. The solvent was distilled off, the residue was dissolved in 40 ml of water and the end product was obtained by lyophilization. Colorless amorphous solid body, decomposition beginning at 128° C, γ C=N1615 cm-1. was separated as an oil The solvent was decanted the product was dissolved in 30 ml of water extracted with 100 ml of ethyl acetate After drying over sodium sulfate the solvent was distilled off under reduced pressure the amorphous residue was dissolved in 30 ml of ethanol The solvent was distilled off the residue was dissolved in 40 ml of water the end product was obtained by lyophilization at 128° C
来源 ID: ord-88cfa64fe19a4ffcab3a66d6a399d3d7反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 5.3 g of 2,4'-dichloro-3'-sulfamoylacetophenone and 3.2 g of ground 1,3-dipropylthio urea were heated in 45 ml of methanol for 5 minutes to 50° C and stirred for another 30 minutes at room temperature. After pouring the reaction mixture into 120 ml of diethyl ether the end product was obtained as a visquous mass which crystallized under mild heating rapidly with ether. Colorless solid body: melting point: 175° C (decomposition). was obtained as a visquous mass which crystallized under mild heating rapidly with ether
来源 ID: ord-7b162885e9c340e1a7fa2adcafa1aa7b反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 5.3 g of 2,4'-dichloro-3'-sulfamoylacetophenone and 3.2 g of ground 1,3-dipropylthio urea were heated in 45 ml of methanol for 5 minutes to 50° C and stirred for another 30 minutes at room temperature. After pouring the reaction mixture into 120 ml of diethyl ether the end product was obtained as a visquous mass which crystallized under mild heating rapidly with ether. Colorless solid body: melting point: 175° C (decomposition). was obtained as a visquous mass which crystallized under mild heating rapidly with ether
来源 ID: ord-7b162885e9c340e1a7fa2adcafa1aa7b反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-e49c56645a554acda01e832be1e74a91反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 6.8 g of 2-bromo-4'-chloro-3'-dimethylsulfamoylacetophenone were reacted according to Example 23 with 3.3 g of 1,3-dipropylthiourea. After adding 200 ml of diethyl ether, 4-(4-chloro-3-dimethylsulfamoylphenyl)-3-propyl-2-propylimino-1,3-thiazolidine-4-ol-hydrobromide was separated as an oil. The solvent was decanted, the product was dissolved in 30 ml of water and extracted with 100 ml of ethyl acetate. After drying over sodium sulfate, the solvent was distilled off under reduced pressure, the amorphous residue was dissolved in 30 ml of ethanol and acidified with ethanolic hydrochloric acid. The solvent was distilled off, the residue was dissolved in 40 ml of water and the end product was obtained by lyophilization. Colorless amorphous solid body, decomposition beginning at 128° C., γ C=N 1615 cm-1. was separated as an oil The solvent was decanted the product was dissolved in 30 ml of water extracted with 100 ml of ethyl acetate After drying over sodium sulfate the solvent was distilled off under reduced pressure the amorphous residue was dissolved in 30 ml of ethanol The solvent was distilled off the residue was dissolved in 40 ml of water the end product was obtained by lyophilization at 128° C.
来源 ID: ord-d7a20ada732648f2bcbd8bf7815b632b反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 5.3 g of 2,4'-dichloro-3'-sulfamoylacetophenone and 3.2 g of ground 1,3-dipropylthio urea were heated in 45 ml of methanol for 5 minutes to 50° C. and stirred for another 30 minutes at room temperature. After pouring the reaction mixture into 120 ml of diethyl ether the end product was obtained as a visquous mass which crystallized under mild heating rapidly with ether. Colorless solid body: melting point: 175° C. (decomposition). was obtained as a visquous mass which crystallized under mild heating rapidly with ether
来源 ID: ord-ed3f76d6e7b847178abb6dfd7f45ceaf反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 2-Chloro-3-quinoxalinecarboxylic acid ethyl ester (3.551 g., 0.015 mole) and 2.405 g. (0.015 mole) of 1,3-di-n-propylthiourea were dissolved in acetone and heated at reflux for 11/2 hours. The solution was concentrated to a volume of 50 ml. and cooled. A small amount of solid was removed by filtration. The filtrate was further concentrated to a volume of 25 ml. and ether was added to turbidity. After the reaction mixture had been cooled the yellow solid was collected by filtration to give 2.77 g. (46.6%) of the product, m.p. 129°-130° C. heated at reflux for 11/2 hours The solution was concentrated to a volume of 50 ml and cooled A small amount of solid was removed by filtration The filtrate was further concentrated to a volume of 25 ml and ether was added to turbidity After the reaction mixture had been cooled the yellow solid was collected by filtration to give 2.77 g
来源 ID: ord-fa6568838bfc4132b2fd45d569acd97c反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 6.8 of 2-bromo-4'-chloro-3'-dimethylsulfamoylacetophenone were reacted according to Example 23 with 3.3 g of 1,3-dipropylthiourea. After adding 200 ml of diethyl ether, 4-(4-chloro-3-dimethylsulfamoylphenyl)-3-propyl-2-propylimino-1,3-thiazolidine-4-ol-hydrobromide was separated as an oil. The solvent was decanted, the product was dissolved in 30 ml of water and extracted with 100 ml of ethyl acetate. After drying over sodium sulfate, the solvent was distilled off under reduced pressure, the amorphous residue was dissolved in 30 ml of ethanol and acidified with ethanolic hydrochloric acid. The solvent was distilled off, the residue was dissolved in 40 ml of water and the end product was obtained by lyophilization. Colorless amorphous solid body, decomposition beginning at 128° C, γ C=N1615 cm-1. was separated as an oil The solvent was decanted the product was dissolved in 30 ml of water extracted with 100 ml of ethyl acetate After drying over sodium sulfate the solvent was distilled off under reduced pressure the amorphous residue was dissolved in 30 ml of ethanol The solvent was distilled off the residue was dissolved in 40 ml of water the end product was obtained by lyophilization at 128° C
来源 ID: ord-88cfa64fe19a4ffcab3a66d6a399d3d7反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 5.3 g of 2,4'-dichloro-3'-sulfamoylacetophenone and 3.2 g of ground 1,3-dipropylthio urea were heated in 45 ml of methanol for 5 minutes to 50° C and stirred for another 30 minutes at room temperature. After pouring the reaction mixture into 120 ml of diethyl ether the end product was obtained as a visquous mass which crystallized under mild heating rapidly with ether. Colorless solid body: melting point: 175° C (decomposition). was obtained as a visquous mass which crystallized under mild heating rapidly with ether
来源 ID: ord-7b162885e9c340e1a7fa2adcafa1aa7bPubChem References
以下资料来自该化合物的公开数据库参考记录。
