Reaktion #1989791

Reaktionsgleichung

4-chloro-1-ethyl-6-methyl-1H-pyrazolo[3,4-b]pyridine-5-carboxylic acid ethyl ester

3-hydroxy-n-butylamine

→

product

1-Ethyl-4-(3-hydroxy-n-butylamino)-6-methyl-1H-pyrazolo-[3,4-b]pyridine-5-carboxylic acid ethyl ester

Lösungsmittel

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture was cooled to room temperature
2. 2
   Sonstigethe toluene layer was decanted from the oil that
3. 3
   Sonstigeseparated out
4. 4
   WaschenThe toluene layer was washed with water
5. 5
   Sonstigedried
6. 6
   Einengenconcentrated in vacuo

Vorschrift

2.75 each of 4-chloro-1-ethyl-6-methyl-1H-pyrazolo[3,4-b]pyridine-5-carboxylic acid ethyl ester and 3-hydroxy-n-butylamine are combined with 15.6 ml of dry toluene under N2 and heated at 45° C. for 48 hours. The mixture was cooled to room temperature and the toluene layer was decanted from the oil that separated out. The toluene layer was washed with water and then dried and concentrated in vacuo to yield 3.7 g of product which crystallized on trituration with hexane. This was recrytallized from hexane to yield 1.91 g of white product mp 94.5°-96.5° C.

Quelle