HRID1159499

反应详情

EQUATION

反应方程式

HRID 1159499 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

(R)-(−)-3-pyrrolidinol hydrochloride (Tokyo Kasei Kogyo Co., Ltd.) (50 g) and potassium carbonate (55.8 g) were dissolved in a mixed solvent of acetonitrile (500 mL) and water (100 mL), and acrylonitrile (29 mL) was added dropwise to the solution at room temperature. Subsequently, the mixture was stirred overnight at room temperature. After the completion of the reaction, the solvent was concentrated, and the obtained residue was dissolved in water. Potassium carbonate was added to saturation. The mixture was extracted 3 times with chloroform, and the extract was dried over potassium carbonate. The solvent was concentrated, and the obtained residue was purified by silica gel column chromatography (chloroform:methanol=10:1) to give (R)-3-(3-hydroxypyrrolidin-1-yl)propionitrile (53 g).

WORKUP

后处理

  1. additionwas added dropwise to the solution at room temperature
  2. customAfter the completion of the reaction
  3. concentrationthe solvent was concentrated
  4. dissolutionthe obtained residue was dissolved in water
  5. additionPotassium carbonate was added to saturation
  6. extractionThe mixture was extracted 3 times with chloroform
  7. dry with materialthe extract was dried over potassium carbonate
  8. concentrationThe solvent was concentrated
  9. customthe obtained residue was purified by silica gel column chromatography (chloroform:methanol=10:1)