5-AMino-4-chloro-2-fluoro-benzoic acid Methyl ester synthesis
- Product Name:5-AMino-4-chloro-2-fluoro-benzoic acid Methyl ester
- CAS Number:716362-14-0
- Molecular formula:C8H7ClFNO2
- Molecular Weight:203.6
1070893-15-0
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$65.00/100mg
716362-14-0
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$90.00/50mg
Yield:716362-14-0 1.33 g
Reaction Conditions:
with iron;ammonium chloride in methanol;water at 75; for 2 h;
Steps:
6 Example 6 Preparation of Intermediate IIb-3: methyl 5-amino-4-chloro-2-fluorobenzoate
The crude IIb-2 (2.34 g, 10.0 mmol, 1.0 eq) was dissolved in CH3OH (20 mL), and water (5 mL), NH4Cl (2.67 g, 50.0 mmol, 5.0 eq) and Fe powder (2.24 g, 40.0 mmol, 4.0 eq) were added. The resulting mixture was stirred at 75° C. for 2 h, and the completion of the reaction was monitored by TLC. After cooling to ambient temperature and concentrating, the filter cake was washed 5 times with CH3OH, and the filtrate was concentrated. The crude product was separated on a silica gel column (EtOAc (ethyl acetate/PE (petroleum ether)=1/2) to obtain 1.33 g (yield 65.5%) of IIb-3 as a yellow solid. LC-MS MS-ESI (m/z) 204.2 [M+H]+.
References:
US2021/139454,2021,A1 Location in patent:Paragraph 0148-0149
35112-05-1
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$13.30/250mg
716362-14-0
24 suppliers
$90.00/50mg