Table 1.
| ||
---|---|---|
Entry | Condition (12→13) | Results |
1 | ~30% yield, incomplete reaction | |
2 | TMSCH2MgBr, THF followed by NaH | ~35% yield, incomplete reaction |
3 | CH2Br2, Zn, TiCl4 THF-CH2Cl2, | 76% yield, 3 d |
4 | Nysted’s Reagent TiCl4, THF-CH2Cl2 | 88% yield, 4 h |