Synthesis · Exceptionally high charge mobility in phthalocyanine-based poly(benzimidazobenzophenanthroline)-ladder-type two-dimensional conjugated polymers

4 structured synthesis routes

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

Complete recipeSource: SI

Route 1: Solvothermal

Methods · Synthesis of 2DCP-MPcs

Metal precursorsoctaaminophthalocyaninato copper(II) hydrochloride, 4-M.8HCl (M = Cu)

Linker precursorsnaphthalenetetracarboxylic dianhydride (1)

SolventsDMI/o-dichlorobenzene (0.50/0.25 mL for film preparation)

AdditivesPTSA catalyst; piranha-cleaned fused silica substrate

Atmospheresame sealed-vacuum polycondensation mixture as powder route

Temperature200

Time120

Substrate orientationfused silica substrate placed vertically in reaction mixture

Work-upFilm washed by immersing in DMF and then acetone; each solvent changed three times.

Activationnatural drying after washing

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	4-M.8HCl (M = Cu)	8.0 mg, 8.1 umol	Methods · Synthesis of 2DCP-MPcs
Linker	naphthalenetetracarboxylic dianhydride (1)	4.3 mg, 16.0 umol	Methods · Synthesis of 2DCP-MPcs
Acid	PTSA	6.2 mg, 32.6 umol	Methods · Synthesis of 2DCP-MPcs
Solvent	DMI/o-dichlorobenzene	0.50/0.25 mL	Methods · Synthesis of 2DCP-MPcs
Other	fused silica substrate	piranha cleaned at 120 C for 5 h	Methods · Synthesis of 2DCP-MPcs

Complete recipeSource: Both

Route 2: Solvothermal

Methods · Synthesis of 2DCP-MPcs

Metal precursorsoctaaminophthalocyaninato copper(II) hydrochloride, 4-M.8HCl (M = Cu)

Linker precursorsnaphthalenetetracarboxylic dianhydride (1)

SolventsDMI/o-dichlorobenzene (0.4/0.2 mL)

AdditivesPTSA catalyst

Atmospheredegassed by three freeze-pump-thaw cycles; sealed under vacuum

Temperature200

Time120

Work-upFiltered; sequentially washed with DMF, DMSO, H2O, ethanol and acetone; Soxhlet extraction with THF 4 h, ethanol 8 h and diethyl ether 2 h.

Activationdried under vacuum at 150 C overnight

Scalability context~90% yield for 2DCP-MPc powder reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	4-M.8HCl (M = Cu)	8.0 mg, 8.1 umol	Methods · Synthesis of 2DCP-MPcs
Linker	naphthalenetetracarboxylic dianhydride (1)	4.3 mg, 16.0 umol	Methods · Synthesis of 2DCP-MPcs
Acid	PTSA	6.2 mg, 32.6 umol	Methods · Synthesis of 2DCP-MPcs
Solvent	DMI/o-dichlorobenzene	0.4/0.2 mL	Methods · Synthesis of 2DCP-MPcs

Complete recipeSource: SI

Route 3: Solvothermal

S6 · Synthesis of 2DCPs and related model compounds

Metal precursorsoctaaminophthalocyaninato nickel(II) hydrochloride, 4-M.8HCl (M = Ni)

Linker precursorsnaphthalenetetracarboxylic dianhydride (1)

SolventsDMI/o-dichlorobenzene (0.50/0.25 mL for film preparation)

AdditivesPTSA catalyst; piranha-cleaned fused silica substrate

Atmospheresame sealed-vacuum polycondensation mixture as powder route

Temperature200

Time120

Substrate orientationfused silica substrate placed vertically in reaction mixture

Work-upFilm washed by immersing in DMF and then acetone; each solvent changed three times.

Activationnatural drying after washing

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	4-M.8HCl (M = Ni)	8.0 mg, 8.1 umol	S6 · Synthesis of 2DCPs and related model compounds
Linker	naphthalenetetracarboxylic dianhydride (1)	4.3 mg, 16.0 umol	S6 · Synthesis of 2DCPs and related model compounds
Acid	PTSA	6.2 mg, 32.6 umol	S6 · Synthesis of 2DCPs and related model compounds
Solvent	DMI/o-dichlorobenzene	0.50/0.25 mL	S6 · Synthesis of 2DCPs and related model compounds
Other	fused silica substrate	piranha cleaned at 120 C for 5 h	S6 · Synthesis of 2DCPs and related model compounds

Complete recipeSource: Both

Route 4: Solvothermal

S5-S6 · Synthesis of 2DCPs and related model compounds

Metal precursorsoctaaminophthalocyaninato nickel(II) hydrochloride, 4-M.8HCl (M = Ni)

Linker precursorsnaphthalenetetracarboxylic dianhydride (1)

SolventsDMI/o-dichlorobenzene (0.4/0.2 mL)

AdditivesPTSA catalyst

Atmospheredegassed by three freeze-pump-thaw cycles; sealed under vacuum

Temperature200

Time120

Work-upFiltered; sequentially washed with DMF, DMSO, H2O, ethanol and acetone; Soxhlet extraction with THF 4 h, ethanol 8 h and diethyl ether 2 h.

Activationdried under vacuum at 150 C overnight

Scalability context~90% yield for 2DCP-MPc powder reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	4-M.8HCl (M = Ni)	8.0 mg, 8.1 umol	S5-S6 · Synthesis of 2DCPs and related model compounds
Linker	naphthalenetetracarboxylic dianhydride (1)	4.3 mg, 16.0 umol	S5-S6 · Synthesis of 2DCPs and related model compounds
Acid	PTSA	6.2 mg, 32.6 umol	S5-S6 · Synthesis of 2DCPs and related model compounds
Solvent	DMI/o-dichlorobenzene	0.4/0.2 mL	S5-S6 · Synthesis of 2DCPs and related model compounds