Reaktion #2075736

Reaktionsgleichung

2-(4-Chloro-2-fluoro-3-methoxyphenyl)-7-methyl-7H-purine-6-carboxylic acid methyl ester

HCl

ethyl acetate

→

title compound

Ausbeute 53.7%

6-Amino-2-(4-chloro-2-fluoro-3-methoxyphenyl)-5-methylaminopyrimidine-4-carboxylic acid

Ausbeute 53.7%

Lösungsmittel

sodium hydroxide

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturheated
2. 2
   Temperaturat reflux for 2 h
3. 3
   TemperaturAfter cooling
4. 4
   workup.DISSOLUTIONThe precipitated solid was dissolved
5. 5
   WaschenThe combined organic phases were washed with brine
6. 6
   Sonstigedried
7. 7
   Sonstigeevaporated

Vorschrift

2-(4-Chloro-2-fluoro-3-methoxyphenyl)-7-methyl-7H-purine-6-carboxylic acid methyl ester (200 mg, 0.57 mmol) was slurried in 2M sodium hydroxide (10 mL) and heated at reflux for 2 h. After cooling, the pH was adjusted to 4 with 1M HCl. The precipitated solid was dissolved by shaking the mixture with two portions of ethyl acetate (45 mL each). The combined organic phases were washed with brine, dried and evaporated to give the title compound (100 mg, 53% yield): 1HNMR (DMSO-d6) δ 7.62 (dd, 1H), 7.36 (dd, 1H), 7.05 (br s, 2H), 3.97 (m, 1H), 3.91 (s, 3H), 2.17 (s, 3H).

Quelle