反応 #465934

反応方程式

p-chlorobenzaldehyde

morpholine

water

→

product

1-Chloro-4-(dimorpholinomethyl)-benzene

溶媒

methylcyclohexane

反応条件

後処理

1. 1
   その他Over the course of 45 minutes, 8.4 ml of water were removed azeotropically
2. 2
   workup.WAITThe mixture was left
3. 3
   温度to cool with slow stirring
4. 4
   その他At 58° C.
5. 5
   その他very fine crystals slowly precipitated out
6. 6
   温度The mixture was cooled in an ice bath to +5° C
7. 7
   その他After a post-stirring time of 1 hour, the solid which had precipitated out
8. 8
   ろ過was filtered off with suction
9. 9
   洗浄The white product was washed with 2×50 ml of methylcyclohexane
10. 10
    その他dried overnight in a drying cabinet at 20° C.

実験手順

70 g of p-chlorobenzaldehyde and 105 g of morpholine were heated to boiling in 260 g of methylcyclohexane in a water separator. Over the course of 45 minutes, 8.4 ml of water were removed azeotropically. The mixture was left to cool with slow stirring. At 58° C., the solution was seeded, and very fine crystals slowly precipitated out. The mixture was cooled in an ice bath to +5° C. After a post-stirring time of 1 hour, the solid which had precipitated out was filtered off with suction. The white product was washed with 2×50 ml of methylcyclohexane and dried overnight in a drying cabinet at 20° C. and 100 mbar. 129.2 g of product were obtained in the form of white crystals (87% of theory).

出典