ACCEPTED MANUSCRIPT
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4.3 Activation of the gaseous substrates CH3Cl, CHCl2F,
CHClF2, CH2F2
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In a JYoung NMR tube ACF · Et3GeH (20 mg for CH3Cl,
25 mg for CHCl2F, CHClF2, CH2F2) was suspended in
Et3GeH (0.4 mmol for CH3Cl, 0.5 mmol for CHCl2F,
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Note the dissolved amount of gaseous substrates is
limited by their solubility in the solvent. The reaction
1
progress was monitored by H NMR spectroscopy. If the
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reaction is performed in Et3GeH as solvent, C6D6 (0.6 mL)
was condensed to the reaction mixture for NMR
spectroscopic analysis after the reaction was stopped.
Conversions were calculated based on signal integration
of the consumed Et3GeH (C6D6:
δ
= 1.06 (t, 9H, CH3,
= 0.99 (t, 9H,
3JH,H = 7.8 Hz) ppm) into Et3GeCl (C6D6:
δ
CH3, 3JH,H = 6.6 Hz) ppm). TONs were calculated based on
the amount of chlorinated substrate assuming ACF
reveals 1 g/mmol catalytically active sites. [60,67]
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Acknowledgement
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We thank Dr. G. Scholz and Dr. K. Scheurell for
recording the MAS NMR spectra. The DFG (Deutsche
Forschungsgemeinschaft) for financial support and
funding the graduate school “SALSA” (School of
Analytical Science Adlershof) is gratefully acknowledged.
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