反应详情

A mixture of 5B (2.02 g, 10 mmol), 3,4,5-trimethoxytoluene (1.82 g; 10 mmol), P2O5 (10.0 g) and dichloromethane 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 ethers:ethyl acetate, 8:2 v/v) and recrystallized from petrol ether:diisopropylether (1:1 v/v). The solid material is collected by vacuum filtration, washed with cold petrol ether:diisopropylether (1:1 v/v) and dried, yielding white crystals, 0.9 g, (24.6%) mp 72° 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 ethers:ethyl acetate, 8:2 v/v)
6. customrecrystallized from petrol ether:diisopropylether (1:1 v/v)
7. filtrationThe solid material is collected by vacuum filtration
8. washwashed with cold petrol ether:diisopropylether (1:1 v/v)
9. customdried
10. customyielding white crystals, 0.9 g, (24.6%) mp 72° C.