反应详情

A mixture of 2,4-dimethoxy 3-methyl benzaldehyde (3.75 g, 20.8 mmole) and beryllium chloride (5.0 g, 62.5 mmole) in anhydrous toluene (50 mL) was heated to reflux for 3.5 hour. The solvent was evaporated under reduced pressure to yield an orange residue, which was treated with 2 N HCl. The compound was extracted with methylene chloride and the organic layer was dried over anhydrous MgSO4. The filtrate was evaporated and dried in vacuo to give an orange solid (3.4 g, 99%): LCMS m/z 168.05 (M+H). 1H NMR (CDCl3/300 MHz) 11.45 (s, 1H), 9.72 (s, 1H), 7.37 (d, 1H, J=8.7 Hz), 6.57 (d, 1H, J=8.7 Hz), 3.92 (s, 3H), 2.10 (s, 3H).

1. temperaturewas heated
2. temperatureto reflux for 3.5 hour
3. customThe solvent was evaporated under reduced pressure
4. customto yield an orange residue, which
5. extractionThe compound was extracted with methylene chloride
6. dry with materialthe organic layer was dried over anhydrous MgSO4
7. customThe filtrate was evaporated
8. customdried in vacuo