A new route to produce acyl radicals by the cleavage of Csp2–Csp2 bonds of α-diketones irradiated by visible light was developed and hydroxylamides or amides were selectively synthesized in water.

We describe a simple and metal‐free photochemical strategy for the direct hydrotrifluoromethylation of vinyl phosphonates or phosphine oxides by sodium triflinate under ultraviolet or visible light irradiation. Acetone and diacetyl were used as radical initiators to generate CF3 radicals that were efficiently added to vinyl phosphonates or phosphine oxide to yield β‐trifluoromethylated phosphorus compounds without the use of any catalyst. A broad scope of substrates scope is demonstrated in moderate to excellent yields. Mechanistic experiments were performed to study the source of hydrogen; the results indicate that H2O in the solvent or additive is the primary hydrogen source.

The photoinduced hydrogenation or deuteration of quaternary arylammonium salts, aryl triflates, and aryl halides under catalyst-free conditions was achieved.

We describe herein a catalyst-free, traditional reductant-free strategy for the direct photoinduced hydrogenation or deuteration of aromatic olefins, ketones, and aldehydes with simple bases as the only additives. A broad...

Rhodamine‐based amide derivatives for the detection of radical intermediates in organic reactions were synthesized and used as fluorescent probes over a wide range of solvents. The mechanistic studies confirm a reversible opening and closing of the spirolactam ring. Compound 21 can be used to support the radical mechanism or in the real‐time monitoring of radical intermediates.