Slfonyl urea compounds and their production method and use
A technology for sulfonylureas and compounds is applied in the fields of sulfonylurea compounds and their preparation and use, and can solve problems such as damage to subsequent crops
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Embodiment 1
[0073] Example 1: Preparation of 2-amino-5-bromo-4-methylpyrimidine (VI).
[0074] Weigh 1.09g (about 0.01mol) of 2-amino-4-methylpyrimidine (III) into a 100ml round bottom flask, add 40ml of dichloromethane or acetic acid, and then add 0.38ml of liquid bromine (about 0.008mol) , the reaction solution was brownish red. The reaction temperature is 20-80 degrees, stirring for 0.5-2 hours. Remove the solvent and add lye to neutralize. CH 2 Cl 2 Extraction, the extract was washed with saturated NaCl. dry (anhydrous Na 2 SO 4 ). Column chromatography (40g silica gel H, 5% CH 3 OH / CH 2 Cl 2 elution) to obtain 0.7 g of white solid. The yield was 50%. TLC (2%CH 3 OH / CH 2 Cl 2 ) Rf = 0.11. [ 1 H] NMR (CD 3 Cl): δ8.19 (s, 1H, Pm), 5.00 (br.s, 2H, NH2), 2.41 (s, 3H, CH3). mp.170-175°C.
[0075] According to the method of Example 1, the compound of general structural formula (VI) of the present invention can be prepared. Example 2: Preparation of 2-amino-5-bromo-4-bro...
Embodiment 2
[0076] Weigh 1.09g (about 0.01mol) of 2-amino-4-methylpyrimidine (III) into a 100ml round bottom flask, add 40ml of dichloromethane or acetic acid, and then add 0.76ml of liquid bromine (about 0.015mol) , the reaction solution was brownish red. The reaction temperature remains between 20-80 degrees. After stirring for 0.5-2 hours, add lye for neutralization. CH 2 Cl 2 Extraction, the extract was washed with saturated NaCl. dry (anhydrous Na 2 SO 4 ). Column chromatography (40g silica gel H, 2% CH 3 OH / CH 2 Cl 2 elution) to obtain 1.4 g of white solid. Yield 52%[ 1 H] NMR (200MHz, CD 3 Cl): δ8.31(s, 1H, Pm), 5.09(br.s, 2H, NH2), 4.36(s, 2H, CH2).mp.184℃(decomposition)
Embodiment 3
[0077] Example 3: Preparation of 2-amino-5-bromo-4-methoxymethylpyrimidine (V).
[0078] Weigh 100mg (0.37mmol) of 2-amino-5-bromo-4-bromomethylpyrimidine (IV) and place it in a 50ml round bottom flask weighing 20ml of methanol, add 12mg of metal Na (about 0.52mmol), and reflux for 1- After 2 hours, the solid residue was washed with water after spin-drying, and separated by column chromatography (silica gel H15g, 3% CH 3 OH / CH 2 Cl 2 ) to obtain 60 mg of white solid. Yield 73%. TLC (3%CH 3 OH / CH 2 Cl 2 ) Rf = 0.3. [ 1 H] NMR (300MHz, CD 3 Cl): δ8.258 (s, 1H, Pm), 5.20 (br.s, 1H, NH2), 4.51 (s, 2H, CH2), 3.53 (s, 3H, CH3). mp.211-215°C.
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