2,3-difluoro-N-methylbenzamide synthesis
- Product Name:2,3-difluoro-N-methylbenzamide
- CAS Number:1250397-72-8
- Molecular formula:C8H7F2NO
- Molecular Weight:171.14
Yield:-
Reaction Conditions:
in tetrahydrofuran at 0; for 0.333333 h;
Steps:
15
A mixture of 2,3-difluorobenzoic acid (1 g, 6.32 mmol) and thionyl chloride (9 mL, 123.53 mmol) is stirred and heated at reflux for 2h. The solvent is evaporated in vacuo and the residue is coevaporated with toluene. Once dried, the residue is dissolved in 5 mL of tetrahydrofuran, chilled at 0°C and monomethylamine (6.32 mL, 12.65 mmol) is added. After 20 min the reaction is quenched with water and extracted with ethyl acetate. The organic layer was separated, dried over magnesium sulfate and the solvent evaporated in vacuo to yield 790 mg of the title compound. MS (m/z): 172 (M+l)
References:
ELI LILLY AND COMPANY;BENITO COLLADO, Ana Belen;DIAZ BUEZO, Nuria;JIMENEZ-AGUADO, Alma Maria;LAFUENTE BLANCO, Celia;MARTINEZ-GRAU, Maria Angeles;PEDREGAL-TERCERO, Concepcion;TOLEDO ESCRIBANO, Miguel Angel WO2011/60217, 2011, A1 Location in patent:Page/Page column 25
4519-39-5
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