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ChemicalBook CAS DataBase List SPIROMESIFEN
283594-90-1

SPIROMESIFEN synthesis

9synthesis methods
7065-46-5 Synthesis
3,3-Dimethylbutyryl chloride

7065-46-5
267 suppliers
$27.00/5g

148476-30-6 Synthesis
4-Hydroxy-3-mesityl-1-oxaspiro(4.4)non-3-en-2-one

148476-30-6
27 suppliers
$180.00/10mg

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Yield:283594-90-1 88%

Reaction Conditions:

with triethylamine in toluene at 0 - 30; for 3 h;

Steps:

2 Synthesis of spiromesifen

272.0 g (1.0 mol) of 3-(2,4,6-trimethylphenyl)-2-oxo-1-oxaspiro[4,4]non-3-en-4-ol dissolved in 800 mL of toluene In solution,Join3,3-dimethylbutyryl chloride 148.0 g (1.1 mol),At 0-10 ° C,111.1 g (0.6 mol) of triethylamine was added dropwise, and a white solid precipitated.After the addition was completed, the temperature was raised to 25-30 ° C, and stirring was continued for 3 hours. The reaction is completed,Cooling, filtering, and removing the resulting triethylamine hydrochloride,Wash with 200 mL of water saturated with sodium carbonate. Then wash with 200ml of water,Dry over anhydrous magnesium sulfate, concentrate,The residue was recrystallized from ethanol to give a white powdery solid (325.6 g,Melting point: 97-98 ° C, yield 88%.

References:

CN109020936,2018,A Location in patent:Paragraph 0027; 0032; 0033

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