反应 #1509657

反应方程式

2,6-dichloro-9-isopropyl-9H-purine

tyramine

triethylamine

→

title compound

4-(2-(2-chloro-9-isopropyl-9H-purin-6-ylamino)ethyl)phenol

溶剂

i-PrOH

反应条件

后处理

1. 1
   浓缩the reaction mixture was concentrated
2. 2
   洗涤was washed with 20% citric acid solution (2.0 L) and water (2.0 L)
3. 3
   浓缩The organic layer was concentrated to dryness
4. 4
   浓缩again concentrated to dryness
5. 5
   其他The crude solid was crystallized from ethanol (3.2 L)

实验过程

2,6-dichloro-9-isopropyl-9H-purine (500 g) was added in portions to a stirred mixture of tyramine (593 g), triethylamine (262 g), and i-PrOH (5.0 L) at 50° C. The mixture was stirred at that temperature for 4 hr, then the reaction mixture was concentrated. The residue was taken up in isopropyl acetate (6.0 L) and was washed with 20% citric acid solution (2.0 L) and water (2.0 L). The organic layer was concentrated to dryness, then was taken up in ethanol (2.0 L) and again concentrated to dryness. The crude solid was crystallized from ethanol (3.2 L) to provide the title compound as a solid.

来源