Optimization of the BCP Bpin cross-coupling reaction.
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Entry | BCP Bpin | Catalysta | Solv., add. | % 8b | % 7 remainingb |
1c | 7a | cataCXium A G2 | PhMe (0.1 M) | 5 | 71 |
2 | 7a | cataCXium A G2 | PhMe (0.1 M) | 21 | 55 |
3 | 7i | cataCXium A G2 | CPME (0.1 M) | 43 | 46 |
4 | 7i | cataCXium A G2 | CPME (0.4 M) | 55 | 25 |
5 | 7i | Pd(OAc)2/cataCXium A (1 : 2) | CPME (0.4 M) | 62 | 9 |
6 | 7b | Pd(OAc) 2 /cataCXium A (1 : 2) | CPME (0.4 M), Cu 2 O (1.0 equiv.) | 69 (53% IY) | 18 |
7 | 7b | Pd(OAc)2/cataCXium A (1 : 2) | CPME (0.4 M), Cu2O (2.0 equiv.) | 56 | 8 |
CataCXium A: (n-Bu)P(1-Ad)2, di(1-adamantyl)-n-butylphosphine.
AY as determined by 1H NMR analysis of the crude reaction mixture against CH2Br2 as an internal standard.
Reaction performed at 100 °C, 0.1 M.