反应详情

A mixture of 6B (24 g, 10 mmol), 3,4,5-trimethoxytoluene (1.82 g; 10 mmol), P2O5 (10.0 g) and dichloromethane (150 ml) is stirred at room temperature for 16 hours. Subsequently, the dichloromethane is distilled off and the residue is diluted with ethyl acetate. The organic phase is washed with water and concentrated. The residue is purified by column chromatography (petrol ether: ethyl acetate, 8:2 v/v) and recrystallized from diisopropylether. The solid material is collected by vacuum filtration, washed with cold petrol ethers:diisopropylether (1:1 v/v) and dried, yielding white crystals, 2.2 g (54% ), mp 89-91° C.

1. distillationSubsequently, the dichloromethane is distilled off
2. additionthe residue is diluted with ethyl acetate
3. washThe organic phase is washed with water
4. concentrationconcentrated
5. customThe residue is purified by column chromatography (petrol ether: ethyl acetate, 8:2 v/v)
6. customrecrystallized from diisopropylether
7. filtrationThe solid material is collected by vacuum filtration
8. washwashed with cold petrol ethers:diisopropylether (1:1 v/v)
9. customdried
10. customyielding white crystals, 2.2 g (54% ), mp 89-91° C.