Table 1 Optimization of reaction conditionsa
From: Room-temperature defluorination of PTFE and PFAS via sodium dispersion
Entry | X | Solvent | Temp. (°C) | Time (h) | Yield (%)b | Entry | X | Solvent | Temp. (°C) | Time (h) | Yield (%)b |
---|---|---|---|---|---|---|---|---|---|---|---|
1 | 5.0 | 1,4-dioxane | 80 | 24 | 69 | 14 | 3.0 | THF | 25 | 12 | 96 |
2 | 5.0 | triglyme | 80 | 24 | 88 | 15 | 2.0 | THF | 25 | 12 | 97 |
3 | 5.0 | diglyme | 80 | 24 | 87 | 16 | 1.5 | THF | 25 | 12 | 65 |
4 | 5.0 | 1,4-dioxane | 50 | 24 | 74 | 17 | 1.0 | THF | 25 | 12 | 22 |
5 | 5.0 | triglyme | 50 | 24 | 86 | 18c | 2.0 | THF | 25 | 12 | 53 |
6 | 5.0 | diglyme | 50 | 24 | 85 | 19c | 2.0 | THF | 25 | 24 | 80 |
7 | 5.0 | THF | 50 | 24 | 94 | 20d | 2.0 | THF | 25 | 12 | 67 |
8 | 5.0 | THF | 25 | 24 | 90 | 21d | 2.0 | THF | 25 | 24 | 95 |
9 | 5.0 | THF | 25 | 12 | 98 | 22d, e | 2.0 | THF | 25 | 12 | 53 |
10 | 5.0 | THF | 25 | 6 | 74 | 23f | 2.0 | THF | 25 | 12 | 33 |
11 | 5.0 | THF | 25 | 3 | 63 | 24g | 2.0 | THF | 25 | 12 | 0 |
12 | 5.0 | THF | 25 | 1 | 49 | 25 | 2.0 | hexane | 25 | 12 | 64 |
13 | 4.0 | THF | 25 | 12 | 92 | 26 | 2.0 | decane | 25 | 12 | 68 |