反应详情

To a solution of 6.19 g. of 4,7-dimethoxyphthalide in 500 ml. of methylene chloride which is cooled to -60° C. is added 48 ml. of diisobutylaluminum hydride in toluene and the mixture is stirred for one hour, 5 ml. of methanol is added and the solution is allowed to come to ambient temperature. The mixture is then treated with 600 ml. of chloroform and 300 ml. of sodium chloride solution and filtered. The organic layer is dried and the solvent removed to yield a white solid. This is washed with hexane to yield 4,7-dimethoxy-1,3-dihydro-1-isobenzofuranol having a melting point of 156°-158° C.

1. additionis added 48 ml
2. customto come to ambient temperature
3. additionThe mixture is then treated with 600 ml
4. filtrationof sodium chloride solution and filtered
5. customThe organic layer is dried
6. customthe solvent removed
7. customto yield a white solid
8. washThis is washed with hexane