HRID489746

反应详情

EQUATION

反应方程式

HRID 489746 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
4 °C

PROCEDURE

实验过程

Galactaric acid (328.0 mg, 1.56 mmol) and (2R)-(4E)-N-methyl-5-(3-pyridyl)-4-penten-2-amine (600.0 mg, 3.40 mmol) were dissolved in 2-propanol (5 mL) and water (0.2 mL), assisted by heating and sonication. The hot solution was filtered to remove some insoluble material. The solvent was removed on a rotary evaporator, and the residue was dried under high vacuum, producing a cream-colored syrup. The syrup was dissolved in dry 2-propanol (5 mL) and cooled at 4° C. The resulting precipitate was filtered and dried under high vacuum to yield 700 mg (79.7%) of an off-white, crystalline powder, mp 131-134° C.

WORKUP

后处理

  1. temperatureby heating
  2. customsonication
  3. filtrationThe hot solution was filtered
  4. customto remove some insoluble material
  5. customThe solvent was removed on a rotary evaporator
  6. customthe residue was dried under high vacuum
  7. customproducing a cream-colored syrup
  8. filtrationThe resulting precipitate was filtered
  9. customdried under high vacuum
  10. customto yield 700 mg (79.7%) of an off-white, crystalline powder, mp 131-134° C.