HRID489746
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureby heating
- customsonication
- filtrationThe hot solution was filtered
- customto remove some insoluble material
- customThe solvent was removed on a rotary evaporator
- customthe residue was dried under high vacuum
- customproducing a cream-colored syrup
- filtrationThe resulting precipitate was filtered
- customdried under high vacuum
- customto yield 700 mg (79.7%) of an off-white, crystalline powder, mp 131-134° C.