反应详情

The diol (1) (16.2 g) in dimethylformamide (50 ml) is added dropwise to sodium hydride (3.1 g) in dimethylformamide (DMF) (50 ml). The mixture is stirred for 20 minutes and then benzyl chloride (16 g) is added and stirring is continued for a further 18 hours at 70° C. After removing the DMF in vacuo, water is added and the mixture is extracted with ether. The combined extracts are dried (MgSO4) and the solvent is evaporated to give a residue which is distilled under reduced pressure to give the title compound as an oil (16.5 g, ca. 60%), b.p. 140°-145° C./0.03 mm, νmax (film) 3440 and 1600 cm-1.

1. stirringstirring
2. waitis continued for a further 18 hours at 70° C
3. customAfter removing the DMF in vacuo, water
4. additionis added
5. extractionthe mixture is extracted with ether
6. dry with materialThe combined extracts are dried (MgSO4)
7. customthe solvent is evaporated
8. customto give a residue which
9. distillationis distilled under reduced pressure