Table 1.
| |||||
---|---|---|---|---|---|
entry | n-Bu4NI (equiv) | solvent | temp (°C) | time (h) | % yielda |
1 | 1 | CH2Cl2 | rt | 60 | 86 (3a) |
2 | 1 | (CH2Cl)2 | 70 | 5 | 90 (3a) |
3 | 0.5 | (CH2Cl)2 | 70 | 5 | 48 (3a) + 45 (2) |
Isolated yields after column chromatography.
| |||||
---|---|---|---|---|---|
entry | n-Bu4NI (equiv) | solvent | temp (°C) | time (h) | % yielda |
1 | 1 | CH2Cl2 | rt | 60 | 86 (3a) |
2 | 1 | (CH2Cl)2 | 70 | 5 | 90 (3a) |
3 | 0.5 | (CH2Cl)2 | 70 | 5 | 48 (3a) + 45 (2) |
Isolated yields after column chromatography.