反应详情

A solution of butyl lithium (0.05 mole) in hexane (34.4 ml), was treated with 2,2,6,6-tetramethylpiperidine (9.3 ml) followed by dry THF (100 ml) under an inert atmosphere at 0° C. The mixture was treated with N-methylcaprolactam (6.9 ml, 55 mM) and stirred for 30 minutes. A solution of butyl lithium (0.05 mole) in hexane (34.4 ml) was added, the reaction mixture stirred 15 minutes then treated with o-chloroanisole (3.1 ml). After 30 minutes a solution of butyl lithium (0.05 moles) in hexane (31.25 ml) was added, the mixture stirred for 15 minutes and treated with o-chloroanisole (3.1 ml). After a further 30 minutes, the reaction was quenched with water (100 ml) and the solvents removed under reduced pressure. The residue was partitioned between 5 N HCl (100 ml) and toluene (250 ml). The organic phase was washed with brine, dried and the solvents removed under reduced pressure.

1. stirringthe reaction mixture stirred 15 minutes
2. stirringthe mixture stirred for 15 minutes
3. waitAfter a further 30 minutes
4. customthe reaction was quenched with water (100 ml)
5. customthe solvents removed under reduced pressure
6. customThe residue was partitioned between 5 N HCl (100 ml) and toluene (250 ml)
7. washThe organic phase was washed with brine
8. customdried
9. customthe solvents removed under reduced pressure