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ChemicalBook CAS DataBase List Isoproturon

Isoproturon synthesis

5synthesis methods
-

Yield:34123-59-6 76%

Reaction Conditions:

Stage #1:4-isopropylphenylisocyanate;N,N-dimethylammonium chloride in tetrachloromethane for 0.333333 h;Inert atmosphere;
Stage #2: with triethylamine in tetrachloromethane at 20; for 16 h;

Steps:

9 Synthesis of 3- (4-isopropylphenyl) -1,1-dimethylurea (isoproturon))
Dimethylamine hydrochloride was added under nitrogen(303 mg, 3.72 mmol)Was suspended in carbon tetrachloride (5 ml), Stirred for 10 minutes,A solution of 4-isopropylphenyl isocyanate in carbon tetrachloride (2 ml, containing 4-isopropylphenyl isocyanate 500 mg, 3.10 mmol) was slowly added dropwise,Stirring was continued for 20 minutes,A solution of triethylamine in carbon tetrachloride (2 ml, containing 627 mg, 6.20 mmol of triethylamine) was slowly added dropwise. After completion of the dropwise addition,20 reaction 16h,The whole reaction was carried out under nitrogen atmosphere,The reaction solution was monitored by TLC,4-isopropylphenyl isocyanate was completely converted, the reaction solution was added with 20 ml of water, and the mixture was stirred three times with 20 ml of dichloromethane,The organic phase was washed with water,Saturated salt water washing,After drying over anhydrous sodium sulfate,Concentrated, concentrated liquid and then recrystallized from dichloromethane, To obtain 486 mg of colorless crystals, yield 76%. (D, 1H, J = 8.0 Hz); 7.14 (d, 3H); 1.21 (s, 3H); 2.13 (s, 2H)See Fig.9

References:

Inspection and Quarantine Technology Center of Hubei Entry - Exit Inspection and Quarantine Bureau;Feng, Yubing;Ni, Lansun;Li, Jing CN106008276, 2016, A Location in patent:Paragraph 0108; 0109; 0110

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