N-substituted (heteroaryl)cycloalkylsulfoximes with insecticidal activity
An alkyl, representative technology, applied in the field of N-substituted (heteroaryl) cycloalkylsulfoxime with insecticidal effect
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Embodiment 1
[0054] Example 1: Methyl (oxidized) (1-[6-(trifluoromethyl)pyridin-3-yl]cyclopropyl)-λ 4 -Preparation of sulfoiminonitrile (1)
[0055]
[0056] To a solution of 3-chloromethyl-6-(trifluoromethyl)pyridine (5.1 g, 26 mmol) in dimethylsulfoxide (DMSO; 20 mL) was added sodium methylthiolate (1.8 g, 26 mmol) in one portion . A violent exotherm was observed, causing the reaction mixture to turn black. The reaction mixture was stirred for 1 hour, then additional sodium methylthiolate (0.91 g, 13 mmol) was added slowly. The reaction mixture was stirred overnight, after which it was poured into H 2 O, add a few drops of concentrated HCl. The mixture was washed with Et 2 O (ether) (3 × 50mL) extraction, combined organic layer, washed with brine, washed over MgSO 4 Dry and concentrate. The crude product was purified by chromatography (Preparative 500, 10% acetone / hexanes) to afford sulfide (A) as a pale yellow oil (3.6 g, 67%). 1 H NMR (300MHz, CDCl 3 )δ8.6(s, 1H), 7.9(d, 1H...
Embodiment II
[0064] Example II: Methyl (oxygen) [1-(6-chloropyridin-3-yl)cyclopropyl]-λ 4 -Preparation of sulfoiminonitrile (2)
[0065]
[0066] Preparation of methyl(oxy)[1-(6-chloropyridin-3-yl)cyclopropyl]-λ from sulfoxime (D) according to the general alkylation conditions described above 4 - Sulfuriminonitrile (2). In the preceding reaction, the precursor sulfoxime (D) was prepared according to the method described in US Patent Application Publication No. 2005 / 0228027A1. The final product was isolated as a colorless oil (32% yield). 1 H NMR (300MHz, CDCl 3 )δ8.6(s, 1H), 8.1(dd, 1H), 7.5(d, 1H), 3.0(s, 3H), 2.3(m, 1H), 2.0(m, 1H), 1.5(m, 2H ); LC-MS (ELSD): C 10 h10 ClN 3 OS[M] + The calculated mass of is 255.72 and the observed value is 255.99.
Embodiment III
[0067] Example III: Methyl (oxygen) [1-(6-chloropyridin-3-yl)cyclobutyl]-λ 4 -Preparation of sulfoiminonitrile (3)
[0068]
[0069] The title compound (3) was prepared from the sulfoxime (D) according to the general alkylation conditions described above. A light brown oil was isolated in 10% yield. 1 H NMR (300MHz, CDCl 3 )δ8.5(d, 1H), 7.8(dd, 1H), 7.5(d, 1H), 3.4(m, 1H), 3.3(m, 1H), 3.0(s, 3H), 2.8(m, 2H ), 2.4(m, 1H), 2.1(m, 1H); LC-MS (ELSD): C 11 h 11 ClN 3 OS[M-H] + The calculated mass of is 268.74 and the observed value is 268.12.
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