反应详情

To a solution of 15.5 g (0.0289 mol) of product of Example 26 in 30 ml of CH2Cl2 cooled in a ice water bath was added 12.0 g of titanium tetrachloride. The reaction mixture turned brown with formation of a white precipitate. After stirring at 10°-15° C. for 20 minutes, then at 20° C. for 20 minutes, the reaction mixture was poured into 70 ml of 6N HCl. The CH2Cl2 layer was separated, dried (MgSO4) and concentrated. The residue was kugelrohr distilled at 2 torr (pot temperature 140° C.) to give 9.1 g (97%) of product as a colorless liquid: nD25 1.4738.

1. waitat 20° C. for 20 minutes
2. customThe CH2Cl2 layer was separated
3. dry with materialdried (MgSO4)
4. concentrationconcentrated
5. distillationThe residue was kugelrohr distilled at 2 torr (pot temperature 140° C.)