HRID47434

反应详情

EQUATION

反应方程式

HRID 47434 的结构方程式

PROCEDURE

实验过程

A stirred mixture of 8-bromo-2-methylquinoline4-carboxylic acid (7.2 g), ethanol (150 ml) and conc. sulfuric acid (3 ml) was boiled for 6 h. After cooling to room temperature solvent was removed at reduced pressure, the residue treated with water and neutralised with solid potassium carbonate. The neutralised mixture was extracted with ethyl acetate, the extracts dried (MgSO4) and solvent removed at reduced pressure. The residue was column chromatographed (silica gel (30% diethyl ether/60-80 petroleum ether) to give the ester (2.5 g). m/z (API+): 294, 296 (MH+).

WORKUP

后处理

  1. customwas removed at reduced pressure
  2. additionthe residue treated with water and neutralised with solid potassium carbonate
  3. extractionThe neutralised mixture was extracted with ethyl acetate
  4. dry with materialthe extracts dried (MgSO4) and solvent
  5. customremoved at reduced pressure
  6. customchromatographed (silica gel (30% diethyl ether/60-80 petroleum ether)