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. 2015 Oct 26;7(1):611–618. doi: 10.1039/c5sc03704b

Table 1. Optimization of Ni-NIXANTPHOS catalyzed DCCP of 1a with 2a a .

Inline graphic
Entry 1a : 2a : base Ni/L (mol%) T (°C) t (h) Concn Yield b (%)
1 1.2 : 1 : 3 10/10 110 16 0.1 78
2 1.2 : 1 : 3 10/15 110 16 0.1 71
3 1.2 : 1 : 3 10/20 110 16 0.1 62
4 1.2 : 1 : 2 10/10 110 16 0.1 83
5 1.2 : 1 : 2 10/10 110 16 0.05 85
6 1 : 1.5 : 2 10/10 110 16 0.05 93
7 1 : 1.5 : 2 10/10 110 8 0.05 77
8 1 : 1.5 : 2 10/10 110 24 0.05 81
9 1 : 1.5 : 2 10/10 50 16 0.05 99
10 1 : 1.5 : 2 10/10 rt 16 0.05 99
11 c 1 : 1.5 : 2 2.5/2.5 rt 16 0.05 99(99)
12 1 : 1.5 : 2 1/1 rt 16 0.05 72

aReactions conducted on a 0.10 mmol scale.

bYield determined by 1H NMR spectroscopy of the crude reaction mixtures.

cIsolated yield after chromatographic purification.