反应详情

2.42 g of 5-(3,4-dibromobutyl)picolinic acid, 2.15 g of dl-α-tocopherol and 4.0 ml of triethylamine were dissolved in 15 ml of methylene chloride, and with stirring under ice cooling, a solution of 1.0 ml of phosphorus oxychloride in 5 ml of methylene chloride was added dropwise. The reaction was performed at this temperature for 3 hours. The reaction mixture was washed with 2 N hydrochloric acid, and then with water, and dried. Then, methylene chloride was distilled off. The residue was chromatographed on a column of silica gel using benzene/ethyl acetate (4:1) as an eluent to give 3.03 g of dl-α-tocopheryl 5-(3,4-dibromobutyl)picolinate as a slightly yellow oil.

1. washThe reaction mixture was washed with 2 N hydrochloric acid
2. dry with materialwith water, and dried
3. distillationThen, methylene chloride was distilled off
4. customThe residue was chromatographed on a column of silica gel