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. 2022 Sep 16;13(39):11623–11632. doi: 10.1039/d2sc02822k

Optimization of reaction conditionsab.

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Entrya PC PC (mol%) Additive Solvent LED Yieldb (%)
1 Xanthone 5.0 MeCN 365 nm 15
2 Thioxanthone 5.0 MeCN 365 nm
3 fac-Ir(ppy)3 5.0 MeCN 365 nm
4 PC 1 5.0 MeCN 365 nm 79
5 PC 2 5.0 MeCN 365 nm 88
6 PC 3 5.0 MeCN 365 nm
7 PC 4 5.0 MeCN 365 nm
8 PC 2 5.0 MeCN 385 nm 90
9 PC 2 5.0 MeCN Blue LED (100 W) 88
10 PC 2 1.0 MeCN 385 nm 83
11 PC 2 2.0 MeCN 385 nm 91 (90) c
12 PC 2 3.0 MeCN 385 nm 81
13 PC 2 4.0 MeCN 385 nm 83
14 PC 2 2.0 THF 385 nm <5
15 PC 2 2.0 DMF 385 nm
16 PC 2 2.0 DCM 385 nm 51
17d PC 2 5.0 DIPEA MeCN 385 nm 29
18d PC 2 5.0 Hantzsch ester MeCN 385 nm
19 MeCN 385 nm
20e PC 2 2.0 MeCN 385 nm
21f PC 2 2.0 MeCN 385 nm 82c
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a

Reaction conditions: 1a (0.1 mmol) and PC (x mol%) were added to degassed MeCN (2.0 mL) under an Ar atmosphere for 12.0 h, in a sealed tube using LED light irradiation.

b

NMR yield using 1,3,5-trimethoxybenzene as an internal standard.

c

Yield of the isolated products.

d

Additive (0.2 mmol) was used.

e

Under dark conditions.

f

A scale-up reaction with 1.0 mmol of 1a.