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3-(CHLOROMETHYL)ISOXAZOLE synthesis

2synthesis methods
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Yield:57684-71-6 78.3%

Reaction Conditions:

with hydroxylamine sulfate in ethanol;Reflux;Solvent;

Steps:

1 Synthesis of 3-chloromethylisoxazole:

Add 400 mL of ethanol to three bottles50.0 g of 1,4-dichloro-3-butenone and 31.0 g of hydroxylamine sulfate.The reaction was heated to reflux and the reaction was monitored by thin layer chromatography.The reaction was poured into 500 mL of ice water, extracted with dichloromethane (100 mL x 3) and the organic phases combined.Washed with saturated sodium bicarbonate, saturated brine, dried over anhydrous sodium sulfate,Under vacuum distillation, 33.1 g (78.3%) of 3-chloromethylisoxazole was collected.

References:

CN103880765,2017,B Location in patent:Paragraph 0021; 0024; 0025; 0036

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