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. 2024 Dec 13;16(3):1411–1416. doi: 10.1039/d4sc07243j

Table 4. Scale-up synthesis and derivatizationsa.

graphic file with name d4sc07243j-u4.jpg
a

Reaction conditions: (a) LiCl (1.0 equiv.), H2O (1.0 equiv.), DMSO, 140 °C; (b) LiAlH4 (5.0 equiv.), THF, 0 °C, then cyclohexanone (1.0 equiv.), PTSA (20 mol%), toluene, reflux; (c) MeMgBr (2.5 equiv.), THF, rt; (d) TFA (5.0 equiv.), DCM, rt; (e) 4CzIPN (2 mol%), Cs2CO3 (1.0 equiv.), DMSO, blue LEDs (30 W); (f) NCS (2.1 equiv.), Fe(OAc)2 (10 mol%), 4,4′-dimethoxy-2,2′-bipyridine (10 mol%), 2,4,6-collidine (1.8 equiv.), CH3CN, purple LEDs (390 nm); (g) NBS (2.1 equiv.), Fe(OAc)2 (10 mol%), 4,4′-dimethoxy-2,2′-bipyridine (10 mol%), 2,4,6-collidine (1.8 equiv.), CH3CN, purple LEDs (390 nm).