反应详情

4.00 g (10.69 mmol) 2,2-bis(4-nitrobenzyl)malonic acid is dissolved in 40 ml tetrahydrofuran and added dropwise in a the course of 2 hours to 64.1 ml (64.1 mmol) of a borane-tetrahydrofuran complex 1.0 M solution in tetrahydrofuran. After 19 hours at 25° C., 50 ml water is carefully added. The reaction mixture is then partitioned between ethyl acetate and water; the organic phase is washed repeatedly with water, dried over sodium sulfate, filtered and concentrated by rotary evaporation. The residue, 3.77 g (97%) of 2,2-bis(4-nitrobenzyl)-1,3-propandiol as white powder is used without further purification.

1. customThe reaction mixture is then partitioned between ethyl acetate and water
2. washthe organic phase is washed repeatedly with water
3. dry with materialdried over sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated by rotary evaporation
6. customThe residue, 3.77 g (97%) of 2,2-bis(4-nitrobenzyl)-1,3-propandiol as white powder is used without further purification