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Chapter 7 159
Buffers: A: water/MeCN/TFA – 95/5/0.1 (%, v/v/v); B: MeCN/water/TFA – 95/5/0.1 (%,
v/v/v)
Gradient: start with 100 % A for 5 min; then in 15 min to 75 % B (i.e. 5 %/min); steady at
75 % B for 2.5 min; drop to 100 % A in 5 min (i.e. 20 %/min); steady at 100 % A for 2.5
min.
Column: Prontosil, RP C18‐AQ, with pre‐column; dimensions: 250 x 4.6 mm (length x
internal diameter), particle size: 5 μm; pore diameter: 120 Å (Knauer, Batch No. 2362,
Column SN: CG 108, 25VF184PSJ).
Detection: λ = 254 nm.
Equipment: HPLC‐runs were performed on a Knauer HPLC‐machine.
7.1.12 Catalytic studies
Catalytical tests for Paal-Knorr reaction in Chapter 4 were performed in collaboration
with the group of Prof. A. Corma, in particular by K. Epp (TU Munich) and Dr. F. X. Llabrés
i Xamena, in the Institute of Chemical Technologies (Instituto de Tecnología Química, ITQ),
Polytechnical University of Valencia (Spain). Ethylene dimerization in Chapter 4 was
carried out by W. Zhang with the assistance of M. Gonzalez (the group of Prof. J. R. Long)
in the department of Chemistry, University of California, Berkeley (US). Catalytic reaction
for the hydrogenation of PNP to PAP in Chapter 5 was performed by Z. Chen and M. Al-
Naji (Group of Prof. R. Gläser) in the institute of Chemical Technology, University of
Leipzig. Data for the catalysis was analyzed by W. Zhang with the assistance of these
collaborators.
Gas Chromatography measurements for monitoring the product of Paal-Knorr reaction
were performed on an Agilent Technologies 7890A with FID (Flame Ionization Detector)
using a capillary column HP-5 (5% phenylmethylpolysiloxane) of 30 m length and 0.32
mm internal diameter as well as BP20(WAX) of 15 m length and 0.32 mm internal
diameter as another column. Thereby, the products were measured in high dilution using
volatile organic solvents (usually ethanol or acetone).