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Page 4 of 9 Wang et al. Chem Synth 2023;3:9 https://dx.doi.org/10.20517/cs.2022.44
Table 1. Condition optimization
Entry a Catalyst Solvent Temp. Time (h) Yield (%) b ee (%) c
1 C1 CH Cl 2 rt 24 60 18
2
2 C2 CH Cl 2 rt 24 47 40
2
3 C3 CH Cl 2 rt 24 14 5
2
4 C4 CH Cl 2 rt 24 13 91
2
5 C5 CH Cl 2 rt 24 30 90
2
6 C6 CH Cl 2 rt 24 9 85
2
7 C7 CH Cl 2 rt 24 13 89
2
8 C5 CHCl 3 rt 36 15 89
9 C5 ClCH CH Cl rt 36 trace -
2
2
10 C5 EtOAc rt 36 trace -
11 C5 toluene rt 36 trace -
12 C5 THF rt 36 trace -
13 C5 MeCN rt 36 20 87
14 C5 CH Cl (0.4 mL) rt 36 35 89
2
2
15 C5 CH Cl (0.3 mL) rt 36 38 89
2
2
16 C5 CH Cl (0.2 mL) rt 36 44 89
2
2
17 C5 CH Cl (0.1 mL) rt 36 52 89
2
2
18 C5 CH Cl (0.05 mL) rt 36 43 89
2
2
19 C5 CH Cl (0.1 mL) rt 72 73 89
2
2
20 C5 CH Cl (0.1 mL) rt 96 78 89
2
2
21 C5 CH Cl (0.1 mL) rt 120 81 89
2
2
22 C5 CH Cl (0.1 mL) rt 144 84 89
2
2
23 d C5 CH Cl (0.1 mL) rt 96 80 89
2
2
e
24 C5 CH Cl (0.1 mL) rt 96 87 89
2
2
25 e C5 CH Cl (0.1 mL) 35 °C 96 90 89
2
2