반응 #67706

반응 방정식

Cyclopropylbromide

magnesium

butyl-[1-(2-fluoro-4,6-bis-trifluoromethyl-phenyl)-methylidene]-amine

intermediate M

butyl-[1-(2-fluoro-4,6-bis-trifluoromethyl-phenyl)-methylidene]-amine

→

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

용매

diethylether

반응 조건

후처리

1. 1
   온도refluxed for 10 min
2. 2
   온도The reaction mixture was refluxed for 2 h
3. 3
   기타The reaction mixture was quenched with 8 mL water
4. 4
   여과filtered through dicalite
5. 5
   기타The organic phase was separated
6. 6
   기타dried on sodium sulfate
7. 7
   여과filtered
8. 8
   기타evaporated
9. 9
   기타The crude material, brown oil (3.54 g, 82%) was used without further purification

실험 절차

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.

출처