HRID750180

反应详情

EQUATION

反应方程式

HRID 750180 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6-Chloro-1-oxo-4-phenyl-1H-isochromen-3-carboxylic acid (150 mg) was dissolved in methanol (3.0 ml) and O-methylhydroxylamine hydrochloride (420 mg) and sodium methoxide (270 mg) were added. The mixture was stirred at room temperature for 12 hrs. and concentrated under reduced pressure. The residue was partitioned between ethyl acetate and 1N hydrochloric acid, and the organic layer was dried over magnesium sulfate and concentrated under reduced pressure to dryness. Then, 4N hydrochloric acid ethyl acetate solution (3 ml) was added to the residue and the mixture was stirred at room temperature for 12 hrs. Water was added to wash the reaction mixture, and the organic layer was dried over magnesium sulfate and concentrated under reduced pressure to give 6-chloro-2-methoxy-1-oxo-4-phenyl-1,2-dihydroisoquinoline-3-carboxylic acid.

WORKUP

后处理

  1. concentrationand concentrated under reduced pressure
  2. customThe residue was partitioned between ethyl acetate and 1N hydrochloric acid
  3. dry with materialthe organic layer was dried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure to dryness
  5. additionThen, 4N hydrochloric acid ethyl acetate solution (3 ml) was added to the residue
  6. stirringthe mixture was stirred at room temperature for 12 hrs
  7. additionWater was added
  8. washto wash the reaction mixture
  9. dry with materialthe organic layer was dried over magnesium sulfate
  10. concentrationconcentrated under reduced pressure