تفاعل #69643

معادلة التفاعل

2,4,5,6-tetrachloropyrimidine

2,4,6-trimethyl aniline

N,N-bis(1-methylethyl)ethanamine

→

4,5,6-trichloro-N-(2,4,6-trimethylphenyl)-2-pyrimidinamine

2,5,6-trichloro-N-(2,4,6-trimethylphenyl)-4-pyrimidinamine

المذيبات

1,4-dioxane

ظروف التفاعل

المعالجة

1. 1
   أخرىThe solvent was evaporated
2. 2
   workup.DISSOLUTIONthe residue was dissolved in CH2Cl2
3. 3
   أخرىpurified by column chromatography over silica gel (eluent: CH2Cl2/hexane ¼, and ½)
4. 4
   أخرىThe desired fractions were collected
5. 5
   أخرىtheir solvent was evaporated

الإجراء التجريبي

2,4,5,6-tetrachloropyrimidine (0.0134 mol), 1,4-dioxane (30 ml), 2,4,6-trimethyl aniline (0.0134 mol), and N,N-bis(1-methylethyl)ethanamine (0.0136 mol) were added to a flask under argon and stirred at 55° C. for 16 hours. The solvent was evaporated, and the residue was dissolved in CH2Cl2, then purified by column chromatography over silica gel (eluent: CH2Cl2/hexane ¼, and ½). The desired fractions were collected and their solvent was evaporated, yielding 0.15 g 4,5,6-trichloro-N-(2,4,6-trimethylphenyl)-2-pyrimidinamine (interm. 6) and 3.15 g 2,5,6-trichloro-N-(2,4,6-trimethylphenyl)-4-pyrimidinamine (interm. 7).

المصدر