Table 1.
Entry | [1] mM | [2] mM | [DBU] mM | time/min | temp/°C | %yieldb |
---|---|---|---|---|---|---|
1 | 100 | 100 | 100 | 5.0 | 75 | 60 |
2 | " | " | " | 5.0 | 100 | 69 |
3 | " | " | " | 7.5 | 75 | 81 |
4 | " | " | " | 7.5 | 100 | 83 |
5 | " | " | " | 10 | 25 | 17 |
6 | " | " | " | 10 | 75 | 85 |
7 | " | " | " | 10 | 100 | 75 |
8 | " | " | " | 12 | 75 | 83 |
9 | " | " | " | 12 | 100 | 81 |
10 | 10 | 100 | 100 | 10 | 75 | 73 |
11 | 100 | 10 | 100 | 10 | 75 | 51 |
12 | 100 | 100 | 10 | 10 | 75 | 10 |
13 | 100 | 100 | 0 | 10 | 75 | 7 |
Reactions (300 μL DMF) were performed in a sealed vessel under a He atmosphere. No carrier added 11CO2 was trapped from a stream of He gas.
See supporting information for details related to radiochemical yield calculation.