반응 #70664

반응 방정식

N2,N7-bis(3-(1,3-dioxolan-2-yl)phenyl)-9,9-dimethyl-N2,N7-di(naphthalen-1-yl)-9H-fluorene-2,7-diamine

hydrochloric acid

→

product

수율 97.3%

3,3′-((9,9-dimethyl-9H-fluorene-2,7-diyl)bis(naphthalen-1-ylazanediyl))dibenzaldehyde

수율 97.3%

용매

acetone

반응 조건

후처리

1. 1
   기타the solvent was removed by evaporation
2. 2
   workup.ADDITION200 mL Ethyl acetate was added
3. 3
   추출the reaction mixture was extracted
4. 4
   건조The organic layer was dried over sodium sulfate
5. 5
   여과After filtration
6. 6
   기타the solvent was removed by evaporation

실험 절차

To a three-neck round-bottom flask, were added 8.0 g N2,N7-bis(3-(1,3-dioxolan-2-yl)phenyl)-9,9-dimethyl-N2,N7-di(naphthalen-1-yl)-9H-fluorene-2,7-diamine and in 100 mL acetone. 41.1 mL 2 M hydrochloric acid solution was added slowly to the reaction mixture through an addition funnel. After TLC showed the reaction was done, the solvent was removed by evaporation. 200 mL Ethyl acetate was added, and the reaction mixture was extracted using DI water (4×200 mL). The organic layer was dried over sodium sulfate. After filtration, the solvent was removed by evaporation. The product (6.9 g) was obtained after drying under vacuum, and was carried on to next step without further purification. The structure was confirmed by NMR.

출처