Table 1.
Dependence of fluorination yield on reaction conditions
entry | solvent | temperature | yield [%] 4 : 13a) |
---|---|---|---|
1 | pyridine | 50 ºC | <1:50 |
2 | 75 ºC | <1:57 | |
3 | 100 ºC | <1:72 | |
4 | DMSO | 50 ºC | 38:60 |
5 | 75 ºC | 48:50 | |
6 | 100 ºC | 66:32 | |
7 | 150 ºC | 97:1 | |
8 | chloroform | 50 ºC | 54:44 |
9 | 75 ºC | 64:33 | |
10 | 100 ºC | 70:27 | |
11 | neat | 75 ºC | 95:<1 |
12 | 100 ºC | 97:<1 | |
13 | 150 ºC | 98:<1 |
Yield determined by 1H and 19F NMR using an internal standard.