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. 2024 Nov 1;14(47):34925–34937. doi: 10.1039/d4ra05774k

Optimization concerning solventa.

graphic file with name d4ra05774k-u3.jpg
Entry Solventbb Reagent Cool white LED (photon flux: 46 μmol s−1) Time (h) Yieldc (%)
1 CH3CN NBS Yes 1 84
2 CH3OH NBS Yes 15 45*
3 CH3CH2OH NBS Yes 15 47*
4 CH3COOCH2CH3 NBS Yes 15 41*
5 CHCl3 NBS Yes 15 27*
6 H2O NBS Yes 15 NA
7 DMSO NBS Yes 15 36*
8 DMF NBS Yes 6 79
9 CH3CN NBS Dark 15 65*
10 CH3OH NBS Dark 15 33*
11 CH3CH2OH NBS Dark 15 40*
12 CH3COOCH2CH3 NBS Dark 15 11*
13 CHCl3 NBS Dark 15 9*
14 DMF NBS Dark 15 38*
15 DMSO NBS Dark 15 21*
16 H2O NBS Dark 15 NA
a

Reaction condition: 1 (0.6 mmol) and NBS were taken in different solvents.

b

Volume of solvent: 1 mL.

c

Pure product was isolated by silica-gel column chromatography, * starting material was not consumed.