반응 #2075736

반응 방정식

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

HCl

ethyl acetate

→

title compound

수율 53.7%

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

수율 53.7%

용매

sodium hydroxide

반응 조건

후처리

1. 1
   온도heated
2. 2
   온도at reflux for 2 h
3. 3
   온도After cooling
4. 4
   workup.DISSOLUTIONThe precipitated solid was dissolved
5. 5
   세척The combined organic phases were washed with brine
6. 6
   기타dried
7. 7
   기타evaporated

실험 절차

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).

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