ChemicalBook CAS DataBase List 2,3-Difluoronitrobenzene

2,3-Difluoronitrobenzene synthesis

4synthesis methods

Product Name:2,3-Difluoronitrobenzene
CAS Number:6921-22-8
Molecular formula:C6H3F2NO2
Molecular Weight:159.09

4519-40-8 Synthesis

4519-40-8
295 suppliers
$10.00/1g

6921-22-8
165 suppliers
$26.00/1g

Yield:6921-22-8 57%

Reaction Conditions:

with dihydrogen peroxide;trifluoroacetic anhydride in dichloromethane;water at 0 - 20;

Steps:

10

To a stirred solution of hydroxy peroxide (30% in H₂O, 35 mL, 356 mmol) under N₂ at0⁰C, a solution of trifluoroacetic anhydride (56 mL, 407 mmol) in 115 mL dichloromethane was added dropwise over 2 h. After addition was complete, a solution of 2,3- difluorobenzenamine (5 g, 39 mmol) in 115 mL dichloromethane was added dropwise at O⁰C. After the addition was complete, the reaction mixture was gradually warmed up to room temperature and stirred overnight. The mixture was extracted by dichloromethane and dried over anhydrous Na₂SO₄. The mixture was filtered and concentrated under reduced pressure. The residue was purified by flash column with 0-15% EtOAc in hexane to yield 3.5 g of 1 ,2- difluoro-3-nitrobenzene (57%). 400 MHz ¹H NMR (CDCI₃) δ (ppm) 7.84 (m, 1H), 7.50 (m, 1H), 7.26 (m, 1H).

References:

WO2008/12623,2008,A1 Location in patent:Page/Page column 62

617-86-7 Synthesis