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3 protocols using 1 3 diphenylurea

1

Synthesis of N-phenyl carbamates

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Methyl N-phenyl carbamate (CAS: 2603-10-3) was purchased from TCI chemicals. Phenyl isocyanate (≥98%), aniline (≥99%), 1,3-Diphenylurea (98%), 1-(2-Pyridyl) piperazine (≥99%), Dimethyl sulfoxide (anhydrous ≥ 99.9%) and diphenyl ether (≥99%) were purchased from Sigma-Aldrich.
Acetonitrile (HPLC grade), water (HPLC grade), ammonium acetate (≥98%), and formic acid (For LC-MS 98–100%) were all purchased from Sigma-Aldrich for use in analytical equipment (LC).
Catalysts include montmorillonite K10 (H2Al2(SiO3)4−nH2O, surface area 220–270 m2/g), zinc oxide (nanopowder, ≤100 nm, 10–25 m2/g), and aluminium oxide (50–300 mesh, acid, 155 m2/g) purchased from Sigma-Aldrich and Bismuth(III) oxide (nanopowder 99.9%, 3.8–5.5 m2/g) was purchased from Fischer scientific. The catalysts were stored in an oven (110 °C) prior to experiments.
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2

Organic Synthesis Reagent Procurement

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Aniline (≥99%), 1,2-dichlorobenzene (99%), dimethyl sulfoxide (>99%), 1,3-diphenyl urea (98%), diphenyl ether (99%), γ -valerolactone (98%), phenyl isocyanate (>98%), and 1-(2-pyridyl)piperazine (>99%) were purchased from Sigma-Aldrich. For the analytical equipment, acetonitrile (HPLC grade), ammonium acetate (>98%), formic acid (for LC-MS 98–100%), and water (HPLC grade) were purchased from Sigma-Aldrich.
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3

HPLC-MS Analysis of Explosives Precursors

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LC-MS grade water containing 0.1 % formic acid, methanol, formic acid, and acetonitrile were purchased from Sigma-Aldrich (Buchs, Switzerland). Diphenylamine was from Fluka (Buchs, Switzerland). Ethylcentralite, N-nitrosodiphenylamine, 4-nitrodiphenylamine, akardite II, 1,3diphenylurea and N,N-diphenylformamide were obtained from Sigma-Aldrich (Buchs, Switzerland).
2-nitrodiphenylamine was from Alfa Aesar (Karlsruhe, Germany). MEthylcentralite was purchased from MP Biomedicals (Illkirch, France).
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