反応 #706588

反応方程式

4-nitrophenyl isothiocyanate

4,4'-diaminodiphenyl methane

→

titled compound

N,N"-(methylenedi-4,1-phenylene)bis[N'-(4-nitrophenyl)thiourea]

溶媒

dioxane

dioxane

反応条件

後処理

1. 1
   その他the solvent is removed by vacuum evaporation
2. 2
   その他The solid obtained
3. 3
   洗浄is washed with n-hexane (3×25 mL) and isopropanol (3×10 mL)
4. 4
   workup.DISSOLUTIONNext, the solid is dissolved in ethyl acetate (50 mL)
5. 5
   洗浄washed with water (3×25 mL)
6. 6
   乾燥The organic phase is dried with sodium sulfate
7. 7
   その他The solvent is removed by vacuum evaporation

実験手順

A solution of 4-nitrophenyl isothiocyanate (0.45 g, 2.52 mmol) in dioxane (25 mL) is slowly added, with magnetic stirring, to a solution of 4,4'-diaminodiphenyl methane (0.25 g, 1.26 mmol) in dioxane (10 mL). After 24 hours of stirring at room temperature, the solvent is removed by vacuum evaporation. The solid obtained is washed with n-hexane (3×25 mL) and isopropanol (3×10 mL). Next, the solid is dissolved in ethyl acetate (50 mL) and washed with water (3×25 mL). The organic phase is dried with sodium sulfate. The solvent is removed by vacuum evaporation. The titled compound is obtained as a yellow powder. mp: 115° C.

出典