Compound N-fluorobenzamido-N'-phenylthiocarbamide as well as preparation and application thereof
A technology of fluorobenzylamino and fluorobenzylhydrazide, which is applied in the fields of botanical equipment and methods, applications, organic chemistry, etc., can solve problems such as the reduction of arable land area, and achieve energy saving and mild reaction conditions. , the effect of convenient operation
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Embodiment 1
[0036] Embodiment 1, the synthesis of compound N-o-fluorobenzamido-N'-phenylthiourea 2a
[0037] (1) Synthesis of intermediate o-fluorobenzoic hydrazide 1a
[0038] Get 4.2g (30mmol) of 2-fluorobenzoic acid and 50ml of anhydrous methanol, add to a 100ml beaker and mix, then add 3ml of concentrated sulfuric acid (concentration is 98%), and heat to reflux at 70°C to 100°C for 7 ~8h, cooling, with anhydrous Na 2 CO 3 Adjust to neutral (pH=7~8), filter with suction, add 3g (43mmol) of NH 2 NH 2 ·H 2 O (mass concentration 85%), heated to 70 ° C ~ 100 ° C, refluxed 7 ~ 8h, to obtain the intermediate o-fluorobenzoic hydrazide 1a.
[0039] (2) Add 0.4g (2.7mmol) of 2-fluorobenzoic hydrazide and 0.4g (3.0mmol) of phenyl isothiocyanate in an agate mortar, grind intermittently for 3-5 hours, and the reactants are viscous The thick liquid turned into a white solid, and the target product was obtained. Recrystallized from absolute ethanol to obtain pure N-fluorobenzamido-N'-phenylth...
Embodiment 2
[0041] Embodiment 2, the synthesis of compound N-p-fluorobenzamido-N'-phenylthiourea 2b
[0042] (1) Synthesis of intermediate p-fluorobenzoic hydrazide
[0043] Get 4.2g (30mmol) of p-fluorobenzoic acid and 50ml of anhydrous methanol, add them to a 100ml beaker and mix them, then add 3ml of concentrated sulfuric acid (concentration is 98%), and heat to reflux at 70°C to 100°C for 7~ 8h, cooling, with anhydrous Na 2 CO 3 Adjust pH=7~8, filter with suction, add 3g (43mmol) NH to the filtrate 2 NH2 ·H 2 O (mass concentration 85%), heated to 70 ° C ~ 100 ° C, refluxed 7 ~ 8h, to obtain the intermediate fluorobenzoic hydrazide 1b.
[0044] (2) Add 0.4g (2.7mmol) p-fluorobenzoic hydrazide and 0.4g (3.0mmol) phenyl isothiocyanate to an agate mortar, grind intermittently for 3-5 hours, and the reactant is formed from viscous liquid Turn into a white solid, that is, the target product. Recrystallized from absolute ethanol to obtain pure N-p-fluorobenzamido-N'-phenylthiourea 2b. ...
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