XQIATTAAVBLNAN-UHFFFAOYSA-N synthesis
- Product Name:XQIATTAAVBLNAN-UHFFFAOYSA-N
- CAS Number:212631-85-1
- Molecular formula:C7H2BrF3O2
- Molecular Weight:254.99
124-38-9
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Yield:212631-85-1 94.5%
Reaction Conditions:
Stage #1: 1-bromo-2,3,4-trifluorobenzenewith n-butyllithium;diisopropylamine in tetrahydrofuran;hexane at -78; for 2 h;Inert atmosphere;
Stage #2: carbon dioxide in tetrahydrofuran;hexane at 20;Concentration;Reagent/catalyst;Time;
Steps:
9.1; 11.1; 17.1 Step 1: 5-bromo-2,3,4-trifluorobenzoic acid
[0510] To a solution of diisopropylamine (10.14 g, 100.20 mmol) in THF (100 mL) was added -BuLi (40.08 mL, 2.5 M in hexane, 100.20 mmol) at -78 °C under nitrogen atmosphere. The stirring was maintained at this temperature for 1 h. Then a solution of l-bromo-2,3,4- trifluorobenzene (17.62 g, 83.50 mmol) in THF (120 mL) was added. After stirring for 1 h at -78 °C, the mixture was transferred to a bottle with dry ice. The mixture was stirred overnight at room temperature. The reaction was quenched with 10% aqueous HCl and pH was adjusted to 1- 2. The mixture was extracted with ethyl acetate (100 mL x 3). The combined organic extracts were washed with water (100 mL) and brine (100 mL) sequentially, dried over Na2S04, filtered and concentrated under reduced pressure to afford the desired product (20.12 g, 94.5% yield). 1H NMR (400 MHz, DMSO-d6): δ 13.95 (s, 1H), 7.97 (m, 1H).
References:
WO2013/107283,2013,A1 Location in patent:Paragraph 0510; 0535; 0562
176317-02-5
258 suppliers
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212631-85-1
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124-38-9
123 suppliers
$214.00/14L
212631-85-1
33 suppliers
inquiry
61079-72-9
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$6.00/1g
212631-85-1
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