Synthesis · Synthesis and characterization of a novel kind soluble, conjugated, and fluorescent chelate polymer containing fluorene ring in the backbone: Optical, electrical, and electrochemical properties

3 structured synthesis routes

Completeness describes how fully the route could be reconstructed from the main article and supporting information.

Complete recipeSource: Main

Route 1: Other

14 · 2.2. Syntheses of the compounds · Scheme 1a

Linker precursorsFDA (1.740 g, 0.5 x 10^-2 mol); 3,4-dihydroxybenzaldehyde (2.07 g, 1.5 x 10^-2 mol)

Solventsmethanol (50 mL plus 20 mL for aldehyde solution); recrystallisation from acetonitrile

Atmospherenot reported

Temperature60

Time3

Work-upFiltered precipitated Schiff base, recrystallised from acetonitrile, dried in a vacuum desiccator.

Activationvacuum desiccator drying

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	9,9'-bis(4-aminophenyl)fluorene (FDA)	1.740 g, 0.5 x 10^-2 mol	14 · 2.2. Syntheses of the compounds · Scheme 1a
Linker	3,4-dihydroxybenzaldehyde	2.07 g, 1.5 x 10^-2 mol	14 · 2.2. Syntheses of the compounds · Scheme 1a
Solvent	methanol	50 mL + 20 mL	14 · 2.2. Syntheses of the compounds · Scheme 1a

Complete recipeSource: Main

Route 2: Other

14-15 · 2.2. Syntheses of the compounds · Scheme 1b

Metal precursorsCrCl3.6H2O (3.72 g, 1.4 x 10^-2 mol)

Linker precursors3,4-HBA (1.38 g, 1 x 10^-2 mol)

Solventsmethanol (50 mL plus 40 mL for CrCl3.6H2O solution); toluene for precipitation and washing

Atmospherenot reported

Temperature60

Time1

Work-upHalf of the MC-2 methanol solution was precipitated by dropping into 50 mL toluene; product was filtered, washed with toluene (2 x 50 mL), and vacuum oven dried for 24 h.

Activationvacuum oven drying for 24 h; for ICP-AES, MC-2 kept at 150 deg C for 3 h to remove hydrate/absorbed water

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	3,4-HBA	1.38 g, 1 x 10^-2 mol	14-15 · 2.2. Syntheses of the compounds · Scheme 1b
Metal Source	CrCl3.6H2O	3.72 g, 1.4 x 10^-2 mol	14-15 · 2.2. Syntheses of the compounds · Scheme 1b
Solvent	methanol	50 mL + 40 mL	14-15 · 2.2. Syntheses of the compounds · Scheme 1b
Solvent	toluene	50 mL precipitation; 2 x 50 mL wash	14-15 · 2.2. Syntheses of the compounds · Scheme 1b

Complete recipeSource: Main

Route 3: Other

14-15 · 2.2. Syntheses of the compounds · Scheme 1b

Metal precursorsMC-2 methanol solution generated from 3,4-HBA and CrCl3.6H2O

Linker precursorsFDA (1.740 g, 0.5 x 10^-2 mol) in 30 mL methanol; preformed MC-2 Cr-coordinated dialdehyde

Solventsmethanol; toluene for precipitation and washing; acetonitrile for washing

Atmospherenot reported

Temperature60

Time4 total (1 h MC-2 formation plus 3 h FDA reflux)

Work-upPolymer precipitated by dropping reaction mixture into 250 mL toluene; washed with toluene (2 x 50 mL) and acetonitrile (2 x 50 mL); vacuum oven dried for 24 h.

Activationvacuum oven drying for 24 h

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	CrCl3.6H2O	3.72 g, 1.4 x 10^-2 mol	14-15 · 2.2. Syntheses of the compounds · Scheme 1b
Linker	3,4-HBA	1.38 g, 1 x 10^-2 mol	14-15 · 2.2. Syntheses of the compounds · Scheme 1b
Linker	FDA	1.740 g, 0.5 x 10^-2 mol	14-15 · 2.2. Syntheses of the compounds · Scheme 1b
Solvent	methanol	50 mL + 40 mL + 30 mL	14-15 · 2.2. Syntheses of the compounds · Scheme 1b
Solvent	toluene	250 mL precipitation; 2 x 50 mL wash	14-15 · 2.2. Syntheses of the compounds · Scheme 1b
Solvent	acetonitrile	2 x 50 mL wash	14-15 · 2.2. Syntheses of the compounds · Scheme 1b