反应 #2075736

反应方程式

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

HCl

ethyl acetate

→

title compound

收率 53.7%

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

收率 53.7%

溶剂

sodium hydroxide

反应条件

后处理

1. 1
   温度heated
2. 2
   温度at reflux for 2 h
3. 3
   温度After cooling
4. 4
   workup.DISSOLUTIONThe precipitated solid was dissolved
5. 5
   洗涤The combined organic phases were washed with brine
6. 6
   其他dried
7. 7
   其他evaporated

实验过程

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).

来源