cMOF Evidence Base

Synthesis evidence

Pd-Embedded Ti Metal–Organic Framework Nanostructures for Photocatalytic Reductive N-Formylation of Nitroarenes in Water

Kar A.K., Behera A., Srivastava R. · ACS Applied Nano Materials · 2022 · 464-475

2 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Other

p002 / SI pS2 · EXPERIMENTAL; Synthesis of Ti-MOF & Pd/Ti-MOF

Metal precursorsvacuum-dried Ti-MOF; PdCl2 ethanolic solution based on 1, 1.5, and 2 wt% Pd
Solventsethanol
Atmospherenot specified
Temperature80 drying; 120 Ti-MOF pre-drying
Timeovernight stirring after NaBH4 addition
Oxidant / reductantNaBH4 (40 mg in 10 mL ethanol)
Work-upPd-containing precipitate filtered, washed with excess ethanol, and dried in an oven at 80 C.
ActivationTi-MOF vacuum-dried at 120 C prior to Pd loading.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Othervacuum dried Ti-MOFrequired amountp002 / SI pS2 · EXPERIMENTAL; Synthesis of Ti-MOF & Pd/Ti-MOF
Metal SourcePdCl2based on 1, 1.5, and 2 wt % of Pdp002 / SI pS2 · EXPERIMENTAL; Synthesis of Ti-MOF & Pd/Ti-MOF
Solventethanolnot specified for dispersion/PdCl2 solution; 10 mL for NaBH4 solutionp002 / SI pS2 · EXPERIMENTAL; Synthesis of Ti-MOF & Pd/Ti-MOF
ReductantNaBH440 mg · in 10 mL ethanolp002 / SI pS2 · EXPERIMENTAL; Synthesis of Ti-MOF & Pd/Ti-MOF
Complete recipeSource: SI

Route 2: Solvothermal

p002 / SI pS2 · EXPERIMENTAL; Synthesis of Ti-MOF & Pd/Ti-MOF

Metal precursorsTi(O-iPr)4 (2.5 mmol)
Linker precursorsNH2-BDC (3.75 mmol)
SolventsN,N-dimethylformamide (60 mL) and methanol (5 mL)
Atmospherenot specified
Temperature150
Time15
Work-upCooled naturally to room temperature; precipitate filtered; washed three times with DMF and five times with methanol.
ActivationNo separate activation reported for pristine Ti-MOF; vacuum drying at 120 C was applied before Pd loading.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceTi(O-iPr)42.5 mmolp002 / SI pS2 · EXPERIMENTAL; Synthesis of Ti-MOF & Pd/Ti-MOF
LinkerNH2-BDC3.75 mmolp002 / SI pS2 · EXPERIMENTAL; Synthesis of Ti-MOF & Pd/Ti-MOF
SolventN,N-dimethyl formamide60 mLp002 / SI pS2 · EXPERIMENTAL; Synthesis of Ti-MOF & Pd/Ti-MOF
Solventmethanol5 mLp002 / SI pS2 · EXPERIMENTAL; Synthesis of Ti-MOF & Pd/Ti-MOF