HRID906218

反应详情

EQUATION

反应方程式

HRID 906218 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To an ice-cold solution of 4-acetoxy-1-(toluene-4-sulfonyl)-pyrrolidine-2-carboxylic acid ethyl ester (3) (0.65 g, 1.83 mmol) in THF (10 mL) is added LiAlH4 (0.135 g, 3.66 mmol) portion wise. Then the reaction mixture is stirred at room temperature for 1 h. After completion of the reaction, it is cooled to 0° C. and then pH of reaction mixture is adjusted to 3 by adding 6N HCl (0.65 mL). The mixture is concentrated, and the residue is triturated with water (8 mL), the solid precipitated out is filtered, washed with cold water (2×4 mL), and dried under reduced pressure to give compound (4) as white solid.

WORKUP

后处理

  1. customAfter completion of the reaction, it
  2. temperatureis cooled to 0° C.
  3. custompH of reaction mixture
  4. concentrationThe mixture is concentrated
  5. customthe residue is triturated with water (8 mL)
  6. customthe solid precipitated out
  7. filtrationis filtered
  8. washwashed with cold water (2×4 mL)
  9. customdried under reduced pressure