Preparation method and application of a kind of fluorine-containing oxamide homo/heteronuclear compound
A technology of oxamide and metal compounds, applied in the application field of insecticidal active drugs, can solve the problems of unreported insecticidal activity research
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Embodiment 1
[0019] Step 1: Add 10.0mmol of 2-amino-5-fluorobenzoic acid to the reaction vessel, dissolve it with 20ml of tetrahydrofuran, dilute 12.0mmol of ethyl oxalyl chloride with 8ml of tetrahydrofuran and add it dropwise to the above solution, in an ice-water bath Reacted for 1 hour, evaporated by rotary evaporation, washed with cold ethanol, and dried under vacuum to obtain a white powdery solid. Yield: 85%.
[0020] 1H-NMR(400MHz,DMSO)δ14.28(s,1H),12.47(s,1H),8.64-8.60(dd,J=5.2Hz,1H),7.79-7.76(m,1H),7.61-7.56 (m,1H),4.35-4.29(q,2H),1.35-1.31(t,3H)
[0021] Step 2: Dissolve 10.0 mmol of the white powder obtained in the previous step reaction in 30 ml of tetrahydrofuran, dilute 15.0 mmol of N,N-dimethyl-1,3-propanediamine with 20 ml of tetrahydrofuran in an ice-water bath, and then drop by drop The above solution was added, stirred overnight at room temperature, evaporated on a rotary basis, washed successively with cold tetrahydrofuran and cold ethanol, and dried in vacuo to obta...
Embodiment 2
[0047] Step 1: Add 10.0mmol of 2-amino-5-fluorobenzoic acid to the reaction vessel, dissolve it with 20ml of tetrahydrofuran, dilute 12.0mmol of ethyl oxalyl chloride with 8ml of tetrahydrofuran and add it dropwise to the above solution, in an ice-water bath Reacted for 1 hour, evaporated by rotary evaporation, washed with cold ethanol, and dried under vacuum to obtain a white powdery solid. Yield: 85%. 1H NMR (400MHz, DMSO) δ14.28(s, 1H), 12.47(s, 1H), 8.64-8.60(dd, J=5.2Hz, 1H), 7.79-7.76(m, 1H), 7.61-7.56( m,1H),4.35-4.29(q,2H),1.35-1.31(t,3H)
[0048] Step 2: Dissolve 10.0 mmol of the white powder obtained in the previous step reaction in 30 ml of tetrahydrofuran, dilute 15.0 mmol of N,N-dimethyl-1,3-propanediamine with 20 ml of tetrahydrofuran in an ice-water bath, and then drop by drop The above solution was added, stirred overnight at room temperature, evaporated on a rotary basis, washed successively with cold tetrahydrofuran and cold ethanol, and dried in vacuo to o...
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