HRID651599

反应详情

EQUATION

反应方程式

HRID 651599 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

7-Methoxynaphthalene-2-sulfonic acid [1-(1-chloro-isoquinolin-7-ylmethyl)-2-oxopyrrolidin-3-(S)-yl]amide (0.07 g, 0.14 mmol), prepared as described in EXAMPLE 1, Part K, is treated with dioxane (1 mL) and 10% aq. NaOH (3 mL) and heated to reflux for 48 hours. The reaction was cooled, acidified with 1 N HCl and extracted with CH2Cl2. The organic layer is separated, dried and concentrated. The residue is purified by column chromatography eluting with 2.5% MeOH/CH2Cl2. The product fractions are collected, concentrated and precipitated with dilute HCl/ether to yield the title compound (0.041 g, 0.086 mmol).

WORKUP

后处理

  1. temperatureheated
  2. temperatureto reflux for 48 hours
  3. temperatureThe reaction was cooled
  4. extractionextracted with CH2Cl2
  5. customThe organic layer is separated
  6. customdried
  7. concentrationconcentrated
  8. customThe residue is purified by column chromatography
  9. washeluting with 2.5% MeOH/CH2Cl2
  10. customThe product fractions are collected
  11. concentrationconcentrated
  12. customprecipitated with dilute HCl/ether