反应详情

To (1R,2S)-(−)-norephedrine (1 g, 6.61 mmol) in THF (20 mL), triphenylphosphine (1.98 ml, 7.94 mmol), diisopropyl azodicarboxylate (1.401 ml, 7.27 mmol) and triethylamine (2.6 ml, 18.8 mmol) was added anr the rm was stirred at room temperature over night. The solvent was evaporated and the crude material was purified on silica eluting with Heptane/EtPAc 1+4 to EtOAc 100% and EtOAc/MeOH 95+5% the fractions containing product were collected giving 2.5 g of with solid containing lot of P(Ph)3O according to LC/MS. This solid was stirred in hexane (50 ml) O/N and than filtered through a pad of Celite 545 giving 0.6 g of an oil.

1. customThe solvent was evaporated
2. customthe crude material was purified on silica eluting with Heptane/EtPAc 1+4 to EtOAc 100% and EtOAc/MeOH 95+5% the fractions
3. additioncontaining product
4. customwere collected
5. customgiving 2.5 g of with solid
6. filtrationthan filtered through a pad of Celite 545 giving 0.6 g of an oil