Table 1. Screening for optimal reaction conditions a .
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Entry | TCICA (equiv.) | KF (equiv.) | Additive | Temp. (°C) | Yield (%) |
1 | 2.0 | — | — | rt | — |
2 | 2.0 | 5.0 | — | rt | 29 |
3 | 2.0 | 5.0 | 0.1 TFA | rt | 27 |
4 | 4.0 | 5.0 | — | rt | 49 |
5 | 6.0 | 5.0 | — | rt | 79 |
6 | 6.0 | 7.0 | — | rt | 81 |
7 | 6.0 | 3.0 | — | rt | 75 |
8 | 2.0 | 3.0 | — | 50 | 61 |
9 | 4.0 | 5.0 | — | 50 | 62 |
10 | 4.0 | 6.0 | — | 40 | 94 |
11 | 6.0 | 5.0 | — | 40 | 26 b |
aYields determined by 19F NMR using fluorobenzene as an internal standard.
bMeCN not dry.