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. 2020 May 6;11(21):5481–5486. doi: 10.1039/d0sc01763a

Optimization of the reaction parametersa.

graphic file with name d0sc01763a-u1.jpg
Entry Deviation in conditions 3aa/4aab 3aa c (%)
1 None 99 : 1 92
2 L2 was used instead of L1 99 : 1 87
3 L3 was used instead of L1 99 : 1 35
4 L4 was used instead of L1 99 : 1 52
5 L5 was used instead of L1 25 : 1 16
6 L6 was used instead of L1 0
7 L7 was used instead of L1 >5
8 (C7H8)3Mo(CO)3 was used 99 : 1 82
9 THF was used as solvent >5
10 Toluene was used as solvent >5
11 DCE was used as solvent 25 : 1 35
12 iPrOH was used as solvent 99 : 1 77
13 THF/EtOH (5 : 1) as solvent 25 : 1 25
14 DCE/EtOH (5 : 1) as solvent 25 : 1 63
15 Without Mo or L1 0
a

Reaction conditions: Mo-catalyst (10 mol%), ligand (15 mol%), 1a (0.2 mmol), PhSO2Na 2a (0.3 mmol), solvent (1.0 mL, 0.2 M), 60 °C, 24 hours.

b

Determined by 1H-NMR of the crude reaction mixture.

c

Isolated yields.