HRID1595157

反应详情

EQUATION

反应方程式

HRID 1595157 的结构方程式

PROCEDURE

实验过程

A mixture of Compound 1 (7.66 g, 50 mmole), which had been obtained in Preparation Example 1, and a 2 N aqueous solution of sodium hydroxide (37.5 ml, 75 mmole) was refluxed for 2 hours. The reaction mixture was cooled to 0° C., to which 6 N hydrochloric acid was added under stirring to acidify the same. Sodium chloride (15 g) was then added, followed by stirring for 1 hour over an ice-acetone bath. Precipitated crystals were collected. Those crystals were washed with chilled water and then dried under reduced pressure, whereby the title compound (5.77 g) was obtained (yield: 92.2%).

WORKUP

后处理

  1. customhad been obtained in Preparation Example 1
  2. additionwas added
  3. stirringby stirring for 1 hour over an ice-acetone bath
  4. customPrecipitated crystals
  5. customwere collected
  6. washThose crystals were washed with chilled water
  7. dry with materialdried under reduced pressure, whereby the title compound (5.77 g)
  8. customwas obtained (yield: 92.2%)