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. 2022 Oct 17;7(43):39147–39158. doi: 10.1021/acsomega.2c05015

Table 1. Solvent Screening for the Synthesis of 8aa.

2.1.

entry solvent time (h) yieldb (%)
1 CH3CN 24 n.r.
2 IPA 24 27
3 DMF 24 n.r.
4 EtOH 24 70
5 THF 24 n.r.
6 DCM 24 n.r.
7 CHCl3 24 n.r.
8 H2O 24 39
9 MeOH 24 61
10 solvent-free 24 25
11c neat 12 46
12 EtOH:H2O (1:1 v/v: 5 mL) 5.5 78
13 EtOH:H2O (1:1 v/v: 10 mL) 2.5 93
14 EtOH:H2O (1:2 v/v: 10 mL) 5 75
15 EtOH:H2O (2:1 v/v: 10 mL) 7 69
a

Reaction conditions: 5 (1 equiv), 6a (1 equiv), and 7 (1 equiv) at room temperature. 5 mol % catalyst.

b

Yield of the isolated product.

c

60 °C. n.r.—no reaction