HRID1600474

反应详情

EQUATION

反应方程式

HRID 1600474 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. waitthe mixture was left at room temperature for over night
  2. extractionThe product was extracted with CH2Cl2
  3. dry with materialThe CH2Cl2 solution was dried
  4. customleaving a brownish solid
  5. customThe ester was purified by column chromatography
  6. additionfollowed by addition of water
  7. washThe bisphosphonic acid derivative was washed with CH2Cl2
  8. filtrationfiltered
  9. customcollected