反应详情

温度

-30 °C

Suspension of 2,7-dibromonaphthalene (61.4 g, 0.21 mole) in ether (400 ml) was cooled to −30° C., and n-BuLi (1.6M in hexane, 135 ml, 0.21 mole) was added. Reaction mixture was allowed to warm to room temperature, stirred for additional 2.5 h, cooled to −30° C., and CH3I (13.5 ml, 0.21 mole) was added. Reaction mixture was allowed to warm to room temperature, stirred for additional 16 h, treated by water (100 ml). Organic layer was separated, water layer was extracted by ether (6×100 ml). Combined organic fraction was evaporated, giving practically pure solid product. The yield 38.1 g (82%).

1. customReaction mixture
2. temperatureto warm to room temperature
3. temperaturecooled to −30° C.
4. customReaction mixture
5. temperatureto warm to room temperature
6. stirringstirred for additional 16 h
7. customOrganic layer was separated
8. extractionwater layer was extracted by ether (6×100 ml)
9. customCombined organic fraction was evaporated
10. customgiving practically pure solid product