RARECHEM AL BI 1384 synthesis

6synthesis methods

Product Name:RARECHEM AL BI 1384
CAS Number:157372-95-7
Molecular formula:C10H8F2O3
Molecular Weight:214.17

95-92-1 Synthesis

95-92-1
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144025-04-7
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157372-95-7
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Yield:157372-95-7 389 g

Reaction Conditions:

in tetrahydrofuran at -40; for 1 h;

Steps:

1

Under an argon gas atmosphere, To THF (1.0L) solution of magnesium (61.8g, 2.53mol) and iodine (50mg), THF ( 0.7L) solution of 1- bromo-2,4-difluorobenzene (489g, 2.48mol) was dropped over 2.5 hours while maintaining the temperature of the reaction solution to 40 below, and a THF solution of 2,4-difluorophenyl magnesium bromide was prepared. This solution was added dropwise over 2.5 hours to THF (0.25L) solution of diethyl oxalate (363g, 2.43mol) while maintaining the temperature of the reaction solution to -40 below, and the mixture was stirred for 1 hour under ice-cooling. After the reaction was completed, saturated aqueous ammonium chloride (0.5 L) and water (1.5 L) were added to the reaction solution, and extracted with ethyl acetate (0.2L × 3). the combined organic layer was washed with saturated brine (0.5L), and then the organic layer was dried over anhydrous magnesium sulfate (50g). After evaporation of the solvent under reduced pressure from this product, by vacuum distillation, light yellow solid of 2-(2,4-difluorophenyl)-2-oxo ethyl acetate (389 g, yield: 73%) was obtained.

References:

JP2016/56156,2016,A Location in patent:Paragraph 0076

348-57-2 Synthesis