HRID1180099

反应详情

EQUATION

反应方程式

HRID 1180099 的结构方程式

PROCEDURE

实验过程

To a suspension of 2.5 g (8.2 mmoles) of the 6-(1,2,4-triazol-1-ylmethyl)-4,9-dihydro-3H-pyrano[3,4-b]indol-1-on a hydrochloride in 50 ml of methanol were added 0.66 ml (10.2 mmoles) of methanesulphonic acid. The mixture was left under stirring at the reflux temperature for 4 hours. The solvent was evaporated to dryness under reduced pressure, the residue dissolved with 10 ml of a saturated bicarbonate solution and extracted 3 times with ethyl acetate. The combined organic phases were dried and evaporated to dryness and the evaporated solid recrystallised from isopropyl alcohol/heptane to give 2.3 g (94%) of the title ester as a yellow crystalline solid.

WORKUP

后处理

  1. waitThe mixture was left
  2. customThe solvent was evaporated to dryness under reduced pressure
  3. dissolutionthe residue dissolved with 10 ml of a saturated bicarbonate solution
  4. extractionextracted 3 times with ethyl acetate
  5. customThe combined organic phases were dried
  6. customevaporated to dryness
  7. customthe evaporated solid recrystallised from isopropyl alcohol/heptane