Recently, visible-light photoredox catalysis has been the leading efficient access to Nradicals under mild conditions. With their weak N-O bond, hydroxylamine derivatives have recently been exploited as nitrogen-centered radical precursors in visible-light photocatalysis. Thus, 4-trifluoromethylbenzoyl hydrox-amic acid derivative (1a) was used as the model substrate to establish optimal reaction parameters, including the equivalency ). Furthermore, We examined the influence of the light source. 467 nm wavelength LED turned out to be better than 456 nm LED, leading a jump increasing yield (from 47% to 73%, entry 10). Higher equivalent photocatalyst (5%) resulted in 77% yield (entry 11). Reducing the B 2 cat 2 loading from 3.0 to 2.5 equiv. led to a slightly improved yield (81% GC yield, isolated in 73%), and 4.0 equiv. B 2 cat 2 gave significantly lower yield (entry 13), which showed that the product yield is not always proportional to the equivalent of borylating reagent. Decreasing the loading of additive DIPEA, the yield dropped to 54% (entry 14). Control experiments revealed that no borylation product formed in the absence of photocatalyst (entry 15), while absence of light or additive, the yields were also low ( 15%, entry 16-17).