HRID1915000

反应详情

EQUATION

反应方程式

HRID 1915000 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

500 mg of methyl 4-oxo-4H-chromene-2-carboxylate were dissolved in 25 ml of anhydrous methanol at room temperature, and NaBH4 was thereafter added to the solution slowly, until the starting material was no longer detected by TLC (about 300 mg). The solvent was then evaporated and a mixture of 1.1 gram of NaH2PO4.2H2O in 30 ml of water was added to the resulting residue. The pH of the mixture was maintained between 5 and 9, so as to prevent decomposition of chromone. The aqueous solution was washed with chloroform (3×50 ml) and the combined organic extracts were dried over Na2SO4. The solvent was evaporated to give 2-(hydroxymethyl)-4H-chromen-4-one which was used without future purification.

WORKUP

后处理

  1. customThe solvent was then evaporated
  2. additiona mixture of 1.1 gram of NaH2PO4.2H2O in 30 ml of water
  3. additionwas added to the resulting residue
  4. temperatureThe pH of the mixture was maintained between 5 and 9
  5. washThe aqueous solution was washed with chloroform (3×50 ml)
  6. dry with materialthe combined organic extracts were dried over Na2SO4
  7. customThe solvent was evaporated