反应详情

This known intermediate was prepared by a previously unreported method from the known 1-benzoyl glycerol. Thus, 50 g of the latter in a mixture of 500 ml of CH2Cl2 and 25 ml of H2O was treated portion-wise with 80 g of NaIO4 under vigorous stirring at room temperature. After addition, stirring was continued for 2 h after which time 100 g of MgSO4 was added and stirring continued for 30 min. The mixture was filtered, the filtrate evaporated in vacuo and the residue distilled in vacuo to yield 26 g of pure (VII) b.p. 92-94°/0.25 mm. 1H NMR (200 MHz; TMS as internal reference) δ(ppm in CDCl3):

1. additionAfter addition
2. stirringstirring
3. stirringstirring
4. waitcontinued for 30 min
5. filtrationThe mixture was filtered
6. customthe filtrate evaporated in vacuo
7. distillationthe residue distilled in vacuo