反应详情

2,6-dihydroxyanthraquinone (1.19 g, 4.98 mmol) and diethyl(4-bromobutyl)phosphonate (3.0 g, 10 mmol) were heated at 60 ° C. in 5 ml DMF in the presence of 0.8 g of K2CO3 for 72 hours. The solution was extracted with CH2Cl2. The CH2Cl2 solution was dried, leaving a yellow solid. The ester was purified by column chromatography. The bisphosphonate ester was converted to the acid by overnight stirring with 4-fold excess of bromotrimethylsilane in dry dichloromethane followed by addition of water. The bisphosphonic acid derivative was washed with CH2Cl2, filtered and collected.

1. extractionThe solution was extracted with CH2Cl2
2. dry with materialThe CH2Cl2 solution was dried
3. customleaving a yellow solid
4. customThe ester was purified by column chromatography
5. additionfollowed by addition of water
6. washThe bisphosphonic acid derivative was washed with CH2Cl2
7. filtrationfiltered
8. customcollected