Table 1.
Entry | T [°C] | t r [min] | Yield 3 [b] [%] |
---|---|---|---|
1[c] | 85 | 60 | 80 |
2[c] | 100 | 60 | 100 |
3[c] | 110 | 30 | 100 |
4[c] | 125 | 15 | 70 |
5[c] | 150 | 15 | 70 |
6[d] | 100 | 30 | 100 |
7[d] | 100 | 15 | 85 |
[a] See the Experimental Section for the reaction conditions. [b] Conversions were determined by 1H NMR, after evaporation of the solvent. [c] Flow stream A: 2 (1 m) in toluene/DMF (9:1) containing 0.1 equiv imidazole; flow stream B: SOCl2 in toluene (3 m). [d] Flow stream A: 2 in DMF containing 1 % imidazole; flow stream B: neat SOCl2.