Table 1.
Entry | Time (h) | Pd(dba)2/Q-phos (mol %) | BrZnCH2CO2 Et (equiv) | Yield 11b (%) |
---|---|---|---|---|
1 | 12 | 1 | 1.1 | 40 |
2 | 12 | 5 | 1.1 | 52 |
3 | 12 | 1 | 3.0 | 62 |
4 | 1.5 | 1 | 3.0 | 92 |
5b | 1.5 | 5 | 2.0 | 85 |
6 | 1.5 | 10 | 3.0 | 90 |
7 | 1.5 | 20 | 3.0 | 95 |
Reactions were carried out by the method reported.17
Syntheses of 13C-labelled analogues were carried out under these conditions.