تفاعل #66629

معادلة التفاعل

4-chloro-5-(2-isopropyl-4-methoxy-5-methyl-phenoxy)-pyrimidin-2-ylamine

aniline

Methylene chloride

→

5-(2-Isopropyl-4-methoxy-5-methyl-phenoxy)-N4-phenyl-pyrimidine-2,4-diamine

ظروف التفاعل

المعالجة

1. 1
   أخرىwas placed in a sealed tube
2. 2
   أخرىinsoluble solid was removed by filtration through celite
3. 3
   غسيلThe combined methylene chloride filtrate was washed with water
4. 4
   تجفيفdried over anhydrous sodium sulfate
5. 5
   أخرىAfter removal of the drying agent
6. 6
   تركيزthe organic phase was concentrated under reduced pressure
7. 7
   أخرىThe residue was purified with silica gel chromatography (2% methanol in methylene chloride)
8. 8
   أخرىto yield a yellow oily residue, which
9. 9
   أخرىwas further purified with preparative TLC and HPLC (5 to 100% acetonitrile in water with 0.1% trifluoroacetic acid

الإجراء التجريبي

A suspension of 4-chloro-5-(2-isopropyl-4-methoxy-5-methyl-phenoxy)-pyrimidin-2-ylamine (0.043 g, 0.14 mmol) in aniline (4 ml) was placed in a sealed tube and heated at 100° C. over night. Methylene chloride was added and insoluble solid was removed by filtration through celite. The combined methylene chloride filtrate was washed with water and dried over anhydrous sodium sulfate. After removal of the drying agent, the organic phase was concentrated under reduced pressure. The residue was purified with silica gel chromatography (2% methanol in methylene chloride) to yield a yellow oily residue, which was further purified with preparative TLC and HPLC (5 to 100% acetonitrile in water with 0.1% trifluoroacetic acid to yield 5-(2-Isopropyl-4-methoxy-5-methyl-phenoxy)-N4-phenyl-pyrimidine-2,4-diamine, M+H: 365.

المصدر