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. 2020 Aug 24;11:4219. doi: 10.1038/s41467-020-17990-z

Table 1.

Optimization of the transition metal-catalyzed C(CO)−C bonds insertion reaction (reaction conditions: 1a (0.2 mmol), 2a (0.1 mmol), catalyst, and additive (50 mg) in DMF (0.5 mL) at room temperature under air atmosphere for 12 h).

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Entry Catalyst (x mol %) Additive Yield (%)a
1 [RuCl2(p-cymene)]2 (5) 51
2 Rh2(OAc)4 (2) 65
3 AgOAc (10) 60
4 Pd(OAc)2 (10) 0
5 Cu(OAc)2 (10) 0
6 [RhCp*Cl2]2 (2) 24
7 [Rh(cod)Cl]2 (2) Trace
8 Rh2(esp)2 (2) 62
9 0
10 Rh2(OAc)4 (2) 4 Å MS 85
11b Rh2(OAc)4 (2) 4 Å MS 70
12c Rh2(OAc)4 (2) 4 Å MS 81
13 Rh2(OAc)4 (1) 4 Å MS 67
14 Rh2(OAc)4 (5) 4 Å MS 84
15d Rh2(OAc)4 (2) 4 Å MS 80
16e Rh2(OAc)4 (2) 4 Å MS 84

aIsolated yields based on 2a.

b4 Å MS (25 mg) was used.

c4 Å MS (75 mg) was used.

d1 mL of DMF was used.

eReaction was carried out under nitrogen atmosphere. esp: α,α,α′,α′-Tetramethyl-1,3-benzenedipropionic acid.