HRID1180099
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- waitThe mixture was left
- customThe solvent was evaporated to dryness under reduced pressure
- dissolutionthe residue dissolved with 10 ml of a saturated bicarbonate solution
- extractionextracted 3 times with ethyl acetate
- customThe combined organic phases were dried
- customevaporated to dryness
- customthe evaporated solid recrystallised from isopropyl alcohol/heptane