ChemicalBook CAS DataBase List METHYL 3,4-DIFLUOROBENZOATE

METHYL 3,4-DIFLUOROBENZOATE synthesis

9synthesis methods

Product Name:METHYL 3,4-DIFLUOROBENZOATE
CAS Number:369-25-5
Molecular formula:C8H6F2O2
Molecular Weight:172.13

67-56-1 Synthesis

67-56-1
752 suppliers
$7.29/5ml-f

455-86-7 Synthesis

455-86-7
406 suppliers
$5.00/10g

369-25-5
165 suppliers
$13.00/25g

Yield: 84%

Reaction Conditions:

with thionyl chloride at 15; for 16 h;Inert atmosphere;

Steps:

106 Example 106: Synthesis of methyl 3,4-difluorobenzoate (127)
To a mixture of compound 126 (20.0 g, 127 mmol) in MeOH (200 mL) was added dropwise SOCl₂(46.0 g, 380 mmol). Then the reaction was stirred at 15° C. for 16 h. The mixture was concentrated under reduced pressure. The residue was diluted with EA (200 mL), washed with sat. NaHCO₃(2×50 mL), the organic layer was dried over Na₂SO₄, concentrated under reduced pressure and dried in vacuum to give compound 127 as white solid (18.3 g, 84% yield, 99% purity). ¹H NMR (400 MHz, CDCl₃) δ 7.88-7.82 (2H, m), 7.27-7.22 (1H, m), 3.93 (3H, s).

References:

THERAVANCE BIOPHARMA R&D IP, LLC;Kulyk, Svitlana;Owens, Christina;Sullivan, Steven D.E.;Kozak, Jennifer;Hughes, Adam D. US2020/188370, 2020, A1 Location in patent:Paragraph 0479; 0738; 0739

75-91-2 Synthesis