6-Aryloxyacetoxy orange ketones and their application in pesticides
A technology of aryloxyacetoxy orange ketone and compound, applied in the field of herbicides, can solve the problem that 6-aryloxyacetoxy orange ketone compounds have not been disclosed, and achieve high herbicidal activity, high control effect and herbicidal activity improved effect
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Embodiment 1
[0035] Example 1: Preparation of 2,4-dihydroxy-a-chloroacetophenone (A):
[0036] Dissolve 20.0g (181.6mmol) of anhydrous resorcinol and 13.0mL (205.0mmol) of chloroacetonitrile in 300mL of dry diethyl ether, cool the reaction flask below 0°C with an ice-salt bath, stir, and add 12.0g (88.0 mmol) dry molten zinc chloride, continue to pass into dry hydrogen chloride gas for 3h, then seal the reaction bottle, place it in the refrigerator for 1d, and the bottom layer is a red oily substance; continue to pass into dry hydrogen chloride gas for 4h, and then place it in the refrigerator 1d, the bottom layer precipitated out as a pale yellow solid. Filter, wash the filter cake twice with anhydrous ether, then transfer it to a round bottom flask, hydrolyze it with 250mL water at a temperature lower than 100°C until it becomes transparent yellow-brown, put it in the refrigerator for 3h, and precipitate a yellow-brown solid. Filter, dry, and recrystallize from ethanol to obtain 17.2 g ...
Embodiment 2
[0037] Example 2: Preparation of 6-Hydroxy-4'-dimethylaminoaurone (B1):
[0038] Add 2.0g (10.7mmol) A into a round bottom flask filled with ethanol (5mL) and fresh 10% KOH solution (15mL), then add 2.24g (15.0mmol) 4-dimethylaminobenzaldehyde, Stir at room temperature, after the reaction is complete, acidify with 1.0mol / L dilute hydrochloric acid, let stand for 1-3 hours, filter with suction, dry, and recrystallize with dichloromethane and ethanol to obtain 6-hydroxy-4'-dimethylaminoaurone ( B1) 1.86g, yield 61.8%, m.p.178~180°C.
Embodiment 3
[0039] Example 3: Preparation of 6-Hydroxy-3'-Fluorinone (B2):
[0040] Add 2.0g (10.7mmol) A into a round bottom flask filled with ethanol (5mL) and fresh 10% KOH solution (15mL), then add 1.86g (15.0mmol) m-fluorobenzaldehyde, stir at room temperature, After the reaction is complete, acidify with 1.0mol / L dilute hydrochloric acid, let stand for 1-3h, filter with suction, dry, and recrystallize with dichloromethane and ethanol to obtain 2.04g of 6-hydroxy-3'-fluoroorange (B2). Yield 74.4%, m.p.272~274°C.
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