反应详情

First, 6.4 g of pyridinium chlorochromate, 0.48 g of sodium acetate, and 10 ml of methylene chloride were placed in a 200 ml flask. Then, 50 ml of a methylene chloride solution containing 6 g of 2,3-difluoro-4'-(6-hydroxyhexyl)oxybiphenyl obtained in Example 2-(f) was added dropwise to the reaction mixture. The reaction mixture was stirred for 18 hours. The reaction mixture was concentrated. The residue was purified by silica gel column chromatography (eluent: toluene) and recrystallized from a mixed solvent of hexane and acetone to obtain 2.56 g of 2,3-difluoro-4'-(5-formylpentyl)oxybiphenyl (Y: 42.9%). The compound thus obtained had a purity of 95.1% by GC.

1. additionwas added dropwise to the reaction mixture
2. concentrationThe reaction mixture was concentrated
3. customThe residue was purified by silica gel column chromatography (eluent: toluene)
4. customrecrystallized from a mixed solvent of hexane and acetone