反应详情

Triphenylphosphine (4.5 g) in dry MC (20 ml) was added dropwise to the product of stage (i) (3.8 g) and carbon tetrabromide (5.8 g) in dry MC (50 ml) at 0°. The solution was stirred at 0° for 1 h and MC was evaporated. The residue was treated with ER (100 ml), filtered and the filtrate was evaporated. The residue was purified by FCC eluting with CX followed by CX-ER (4:1) to give the title compound as a colourless oil (4.2 g). T.l.c. (CX-ER 9:1) Rf 0.4.

1. customMC was evaporated
2. additionThe residue was treated with ER (100 ml)
3. filtrationfiltered
4. customthe filtrate was evaporated
5. customThe residue was purified by FCC
6. washeluting with CX