Pyrazole oxime derivatives containing dichloropropene and methods for their preparation and application
A technology of dichloropropene and pyrazole oxime is applied in the field of pesticides to achieve excellent control effects
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0033] Synthesis of Compound Ia (n=1, R=3-F)
[0034]
[0035] 5 mmol of compound II was dissolved in an appropriate amount of N,N-dimethylacetamide, and 6 mmol of compound III and 10 mmol of cesium carbonate were added thereto. After heating under reflux for 18h, the reaction was detected by TLC. Filtration, the filtrate was concentrated under reduced pressure, the crude product was dissolved in dichloromethane, washed with water, dried, concentrated, and separated by column chromatography to obtain the target product Ia, a pale yellow oil. 1 H NMR (400MHz, CDCl 3 ) 7.78(s, 1H, CH=N), 7.23-7.29(m, 1H, ArH), 6.78-6.82(m, 3H, ArH), 6.63-6.69(m, 2H, ArH), 6.11(t, J =6.4Hz,1H, CH CH 2 ),4.57(d,J=6.4Hz,2H,CHC H 2 O),4.22(t,J=6.4Hz,2H,CH 2 OAr), 3.99(t, J=6.4Hz, 2H, C H 2 O-N=CH), 3.62(s, 3H, N-CH 3 ),2.38(s,3H,CH 3 ),2.04-2.11(m,2H,CH 2 C H 2 CH 2 ).
Embodiment 2
[0037] Synthesis of Compound Ib (n=1, R=4-F)
[0038]
[0039] Dissolve 5 mmol of compound II in an appropriate amount of acetonitrile, add 6.5 mmol of compound III and 15 mmol of K to it 2 CO 3 . After heating under reflux for 15h, the reaction was detected by TLC. Filtration, the filtrate was concentrated under reduced pressure, the crude product was dissolved in dichloromethane, washed with water, dried, concentrated, and separated by column chromatography to obtain the target product Ib, a pale yellow oil. 1 H NMR (400MHz, CDCl 3 ) 7.78(s, 1H, CH=N), 6.86-7.04(m, 4H, ArH), 6.84(s, 2H, Ar-H), 6.13(t, J=6.0Hz, 1H, C H CH 2 ),4.60(d,J=4.0Hz,2H,CHC H 2 O),4.24(t,J=6.0Hz,2H,C H 2 OAr),4.01(t,J=6.0Hz,2H,C H 2 O-N=CH), 3.63(s, 3H, N-CH 3 ),2.39(s,3H,CH 3 ),2.06-2.13(m,2H,CH 2 C H 2 CH 2 ).
Embodiment 3
[0041] Synthesis of Compound Ic (n=1, R=4-OCF 3 )
[0042]
[0043] 5 mmol of compound II was dissolved in an appropriate amount of N,N-dimethylformamide, and 7 mmol of compound III and 14 mmol of 4-N,N-lutidine were added thereto. After heating under reflux for 20h, the reaction was detected by TLC. Filtration, the filtrate was concentrated under reduced pressure, the crude product was dissolved in dichloromethane, washed with water, dried, concentrated, and separated by column chromatography to obtain the target product Ic, a pale yellow oil. 1 H NMR (400MHz, CDCl 3 )7.70(s,1H,CH=N),7.09(d,J=8.8Hz,2H,ArH),6.84(J=9.2Hz,2H,ArH),6.75(s,2H,Ar-H),6.03 (t,J=8.0Hz,1H,C H CH 2),4.50(d,J=6.4Hz,2H,CHC H 2 O),4.12(t,J=6.4Hz,2H,C H 2 OAr), 3.91(t, J=6.4Hz, 2H, C H 2 O-N=CH), 3.55(s, 3H, N-CH 3 ),2.30(s,3H,CH 3 ),1.95-2.00(m,2H,CH 2 C H 2 CH 2 ).
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More 


