Bromocyclopropane → Butyl-[1-(2-cyclopropyl-4,6-bis-trifluoromethyl-phenyl)-methylidene]-amine

Cyclopropylbromide (3.84 g, 32 mmol) was added to magnesium (771 mg, 32 mmol) in 20 mL diethylether and refluxed for 10 min. Manganese(II) chloride (160 mg, 1.27 mmol) and butyl-[1-(2-fluoro-4,6-bis-trifluoromethyl-phenyl)-methylidene]-amine (intermediate M, 4 g, 13 mmol) was added. The reaction mixture was refluxed for 2 h. The reaction mixture was quenched with 8 mL water and filtered through dicalite. The organic phase was separated and dried on sodium sulfate, filtered and evaporated. The crude material, brown oil (3.54 g, 82%) was used without further purification.

1. temperaturerefluxed for 10 min
2. temperatureThe reaction mixture was refluxed for 2 h
3. customThe reaction mixture was quenched with 8 mL water
4. filtrationfiltered through dicalite
5. customThe organic phase was separated
6. customdried on sodium sulfate
7. filtrationfiltered
8. customevaporated
9. customThe crude material, brown oil (3.54 g, 82%) was used without further purification

ORD-Eintrag

ord-98c6ae645cf442be9c235d2382fa39de

Quelldatensatz

uspto-grants-2013_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08524909B2