反应详情

温度

0 °C

To a stirred solution of compound of formula (1) (1 g, 0.003 mol) in dry toluene (5 ml), diethylzinc (1.1 M solution in toluene, 14 ml, 0.017 mol) was added at 0° C. under nitrogen atmosphere followed by diiodomethane (1.38 ml, 0.017 mol). The reaction was stirred for 16 h at 0° C. and poured over cold aqueous solution of ammonium chloride. The organic layer was separated and the aqueous layer extracted repeatedly with toluene. The combined organic layer was washed with a solution of sodium thiosulphate, dried over anhydrous sodium sulphate, filtered and concentrated to yield racemic betaxolol of formula (2) 1.6 g (84%) mp 70 –72° C. as a white solid.

1. customThe organic layer was separated
2. extractionthe aqueous layer extracted repeatedly with toluene
3. washThe combined organic layer was washed with a solution of sodium thiosulphate
4. dry with materialdried over anhydrous sodium sulphate
5. filtrationfiltered
6. concentrationconcentrated