反应详情

A hexane solution of nBuLi (1.57 M, 1.02 mL) was added dropwise to a THF solution (50 mL) of 2a which had been precooled to −30° C. Once the addition was complete the reaction mixture was allowed to warm to room temperature. After stirring for an additional 12 h the reaction mixture was poured into water and extracted with ether. The ether layer was washed with water and dried with MgSO4. The solvent was removed under reduced pressure. The residue was crystallized from a THF/MeOH mixture at −15° C. to give colorless crystals of 3,3′,4,4′-tetrakisdecyloxybiphenyl (3a) in 38% yield (mp 85-86° C.).

1. customhad been precooled to −30° C
2. additionOnce the addition
3. extractionextracted with ether
4. washThe ether layer was washed with water
5. dry with materialdried with MgSO4
6. customThe solvent was removed under reduced pressure
7. customThe residue was crystallized from a THF/MeOH mixture at −15° C.