Scheme 2.

Optimized conditions and scope of the photocatalytic decarboxylative phosphorylation. Standard conditions: 3 (0.2 mmol), 4 (0.6 mmol), 4CzIPN (2 mol %), trifluoroacetic acid (TFA, 0.3 mmol), in acetonitrile (2.0 mL), 40 W blue LED, 2 h. Three letter code for parent N‐Boc amino acids shown. Yields are of isolated products. ^a Yield of large scale reaction (2.4 mmol); ^b tribenzyl phosphite used; ^c Ir[(dtbppy)(ppy)₂]PF₆ (1 mol %) used; ^d triethyl phosphite used; ^e starting 3 ac d.r.=5 : 1; Cy, cyclohexyl; Xan, xanthenyl; ^f reaction yield (¹H NMR) using conditions from current optimum methodology by Hernández et al. (see Supporting Information for protocol). ^[19]