HRID1510632

反应详情

EQUATION

反应方程式

HRID 1510632 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
66 °C

PROCEDURE

实验过程

To 2.8 g of 1-(1,3-dioxolan-2-ylmethyl)-7-methoxy-1,8-naphthyridin-2(1H)-one, 20 mL of an 80% aqueous trifluoroacetic acid solution was added, and the mixture was stirred at 60 to 72° C. for 3 hours 20 minutes, and at 80 to 85° C. for 2 hours 20 minutes, 4 mL of water was then added thereto and the mixture was further stirred for 4 hours. The reaction mixture was cooled to room temperature and then left overnight, and the solvent was distilled off under reduced pressure. To the resultant residue, a saturated aqueous sodium hydrogen carbonate solution and chloroform were added, the organic layer was separated, and the aqueous layer was extracted with chloroform. The organic layer and the extract were combined, the resultant solution was dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure to obtain 1.8 g of (7-methoxy-2-oxo-1,8-naphthyridin-1(2H)-yl)acetaldehyde as a yellow solid.

WORKUP

后处理

  1. stirringthe mixture was further stirred for 4 hours
  2. temperatureThe reaction mixture was cooled to room temperature
  3. waitleft overnight
  4. distillationthe solvent was distilled off under reduced pressure
  5. additionTo the resultant residue, a saturated aqueous sodium hydrogen carbonate solution and chloroform were added
  6. customthe organic layer was separated
  7. extractionthe aqueous layer was extracted with chloroform
  8. dry with materialthe resultant solution was dried over anhydrous magnesium sulfate
  9. distillationthe solvent was distilled off under reduced pressure