HRID1600474
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
1.34 g of KOH in ethanol were added dropwise to a mixture of 2,6-dihydroxynaphthalene (1.6g, 10 mmol) and diethyl(4-bromobutyl)phosphonate (6.0 g, 22 mmol) in ethanol, the mixture was left at room temperature for over night. The product was extracted with CH2Cl2. The CH2Cl2 solution was dried, leaving a brownish 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.
WORKUP
后处理
- waitthe mixture was left at room temperature for over night
- extractionThe product was extracted with CH2Cl2
- dry with materialThe CH2Cl2 solution was dried
- customleaving a brownish solid
- customThe ester was purified by column chromatography
- additionfollowed by addition of water
- washThe bisphosphonic acid derivative was washed with CH2Cl2
- filtrationfiltered
- customcollected