HRID622198

反应详情

EQUATION

反应方程式

HRID 622198 反应方程式

PROCEDURE

实验过程

17.8 g (74.3 mmol) of the compound (2) thus obtained was added to 50 ml of water, to which 100 ml of methylene chloride was added. This solution was made basic with 25% aqueous solution of sodium hydroxide under water-cooling. The solution was separated and the aqueous layer was extracted with 20 ml of methylene chloride. The obtained methylene chloride layers were combined, washed with 30 ml of water, dried over anhydrous magnesium sulfate and then concentrated under vacuum to obtain 15.06 g of 8-methoxy-6,7-methylenedioxyisoquinoline (3) (yield 99.7%). The product thus obtained was recrystallized from ethylacetate-n-hexane, m.p. 144°-5° C. IR and NMR spectra of the resultant product are listed below. ##STR48##

WORKUP

后处理

  1. additionwas added
  2. temperaturecooling
  3. customThe solution was separated
  4. extractionthe aqueous layer was extracted with 20 ml of methylene chloride
  5. washwashed with 30 ml of water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated under vacuum