1,3-diethylthiourea

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a filtered solution of 1.32 g. of 1,3-diethyl-2-thiourea in 25 ml. of acetone is added a filtered solution of 3-bromo-1,1-diphenyl-2-propanone in 25 ml. of acetone. The mixture is allowed to stand, then the solid is collected by filtration, washed with acetone and dried in vacuo, giving 3.73 g. of the desired product, m.p. 174°-176° C. (dec.). the solid is collected by filtration washed with acetone dried in vacuo giving 3.73 g

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Prepared by the method described in Example 1 from N,N'-diethylthiourea (1.0 g, 8 mmoles) and acetylenedicarboxylic acid (1 g, 9 mmoles). Crystallization from hexane gave the product (1.5 g), mp 148°-152° C. Prepared by the method Crystallization from hexane

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Prepared by the method described in Example 1 from N,N'-diethylthiourea (1.0 g, 8 mmoles) and acetylenedicarboxylic acid (1 g, 9 mmoles). Crystallization from hexane gave the product (1.5 g), mp 148°-152° C. Prepared by the method Crystallization from hexane

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 7.0 g of 3'-di-n-butylsulfamoyl-2,4'-dichloro-acetophenone were reacted according to Example 12 with 2.7 g of 1,3-diethylthiourea and worked up. Colorless solid body, decomposition beginning at 139° C, γ C=N 1615 cm-1. at 139° C

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 6.8 g of 2-bromo-4'-chloro-3'-dimethylsulfamoylacetophenone and 2.7 g of 1,3-diethylthiourea were reacted as prescribed in Example 23. The solvent was decanted and the oily precipitate of the end product was crystallized under fresh acetone. Colorless solid body, decomposition beginning at 154° C, γ C=N 1610 cm-1. The solvent was decanted the oily precipitate of the end product was crystallized under fresh acetone at 154° C

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 6.8 g of 2-bromo-4'-chloro-3'-dimethylsulfamoylacetophenone and 2.7 g of 1,3-diethylthiourea were reacted as prescribed in Example 23. The solvent was decanted and the oily precipitate of the end product was crystallized under fresh acetone. Colorless solid body, decomposition beginning at 154° C, γ C=N 1610 cm-1. The solvent was decanted the oily precipitate of the end product was crystallized under fresh acetone at 154° C

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 7.8 g of 2,4'-dichloro-3'-o-chlorobenzylsulfamoylacetophenone and 2.5 g of 1,3-diethylthiourea were reacted as prescribed in Example 12 and worked up. Colorless crystals, decomposition beginning at 94° C, γ C=N 1615 cm-1. at 94° C

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 7.8 g of 2,4'-dichloro-3'-o-chlorobenzylsulfamoylacetophenone and 2.5 g of 1,3-diethylthiourea were reacted as prescribed in Example 12 and worked up. Colorless crystals, decomposition beginning at 94° C, γ C=N 1615 cm-1. at 94° C

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 6.4 g of 3'-n-butylsulfamoyl-2,4'-dichloroacetophenone and 2.7 g of ground 1,3-diethylthiourea were reacted as prescribed in Example 12. With the addition of 200 ml of diisopropyl ether, the oily end product was precipitated and the solvent was decanted. The amorphous residue was dissolved in 100 ml of water and liophylized. Colorless solid body, decomposition beginning at 130° C, γC=N 1620 cm-1. the oily end product was precipitated the solvent was decanted The amorphous residue was dissolved in 100 ml of water at 130° C

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 5.6 g of 2,4'-dichloro-3'-methylsulfamoylacetophenone and 2.7 g of 1,3-diethylthiourea were reacted as prescribed in Example 12. After the addition of 100 ml of diisopropyl ether and a dwelling period of 1 hour at 0° C, the solvent was decanted and the oily end product was crystallized under boiling diethyl ether. Colorless solid body, melting point: 168° C (decomposition). a dwelling period of 1 hour at 0° C, the solvent was decanted the oily end product was crystallized under boiling diethyl ether

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 5.6 g of 2,4'-dichloro-3'-methylsulfamoylacetophenone and 2.7 g of 1,3-diethylthiourea were reacted as prescribed in Example 12. After the addition of 100 ml of diisopropyl ether and a dwelling period of 1 hour at 0° C, the solvent was decanted and the oily end product was crystallized under boiling diethyl ether. Colorless solid body, melting point: 168° C (decomposition). a dwelling period of 1 hour at 0° C, the solvent was decanted the oily end product was crystallized under boiling diethyl ether