HRID1444748

反应详情

EQUATION

反应方程式

HRID 1444748 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
85 °C

PROCEDURE

实验过程

3-(5-Ammoniopentanoyl)pyridinium chloride (150 mg, 0.60 mmol) and 2-fluorobiphenyl-4-carboxaldehyde (155 mg, 0.78 mmol) were combined in a reaction vessel and treated with ethanol (10 mL) and concentrated HCl(aq) (5 drops). The vessel was then sealed and the reaction was heated to 85° C. overnight then cooled to room temperature. The reaction mixture was then concentrated under reduced pressure then partially dissolved into hot isopropanol. This mixture was left to cool and crystals formed. The crystals were recovered by vacuum filtration, washed with fresh isopropanol, and dried under vacuum giving 92 mg (36%) of a yellow solid. LC-MS: RT=5.88 min, [M+H]+=343.1.

WORKUP

后处理

  1. customThe vessel was then sealed
  2. temperaturethen cooled to room temperature
  3. concentrationThe reaction mixture was then concentrated under reduced pressure
  4. dissolutionthen partially dissolved into hot isopropanol
  5. waitThis mixture was left
  6. temperatureto cool
  7. customcrystals formed
  8. filtrationThe crystals were recovered by vacuum filtration
  9. washwashed with fresh isopropanol
  10. customdried under vacuum