10.1002/adsc.201901253
Advanced Synthesis & Catalysis
Ir[dF(CF3)ppy]2[4,4’-d(CF3)bpy]PF6 (4a, 1.2 mg, 0.001
mmol, 1 mol%), HAT catalyst 5a (4.0 mg, 0.015 mmol, 15
mol%), Martin’s spirosilane (6a, 5.1 mg, 0.01 mmol, 10
mol%), and benzalmalononitrile (1a, 15.4 mg, 0.1 mmol, 1
eq) were added to a dried screw-cap vial. Ethanol (2a, 17.5
L, 0.3 mmol, 3 equiv) and degassed CH3CN (2 mL) were
added to the vial under argon atmosphere in a glovebox.
The vial was sealed with the screw cap. The resulting
mixture was then placed near a light source[23] and
irradiated with blue LED lights while stirring at ambient
temperature for 14 h. After evaporation, the residue was
purified by flash column chromatography to afford 3aa
(18.8 mg, 94 % yield, white solid).
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Acknowledgements
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This work was supported by a JSPS fellowship Grant Number
JP19J23157 (K.S.), JSPS KAKENHI Grant Number JP16H04239
in Precisely Designed Catalysts with Customized Scaffolding and
JSPS KAKENHI Grant Number JP18K06545 in Scientific
Research C (K.O.), JSPS KAKENHI Grant Number JP17H06442
in Hybrid Catalysis (M.K.).
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