HRID2038372

反应详情

EQUATION

反应方程式

HRID 2038372 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.00 g (4.05 mmol) of the compound from Example 21A is provided in 40 ml of acetone, 2.60 g (12.1 mmol) of sodium periodate, 0.70 g (9.11 mmol) of ammonium acetate and 40 ml of water are added and the mixture is stirred at room temperature overnight. The mixture is subsequently concentrated, a 2N aqueous sodium hydroxide solution is added to the residue and the precipitate that remains is filtered off with suction. Using a concentrated aqueous hydrogen chloride solution, the solution is adjusted to pH 3 and cooled to 0° C. The precipitate formed is collected by suction filtration, washed with water and dried under high vacuum. 384 mg (58% of theory) of the title compound are obtained.

WORKUP

后处理

  1. concentrationThe mixture is subsequently concentrated
  2. additiona 2N aqueous sodium hydroxide solution is added to the residue
  3. filtrationthe precipitate that remains is filtered off with suction
  4. temperaturecooled to 0° C
  5. customThe precipitate formed
  6. filtrationis collected by suction filtration
  7. washwashed with water
  8. customdried under high vacuum