تفاعل #42057

معادلة التفاعل

2,4-diaminotoluene

N,N-diisopropyl-N-ethylamine

4-(4-methylpiperazin-1-ylmethyl)-3-trifluoromethylbenzoyl chloride dihydrochloride

→

objective compound

المردود 74.0%

4-(4-methylpiperazin-1-ylmethyl)-3-trifluoromethyl-N-(3-amino-4-methylphenyl)benzamide

المردود 74.0%

المذيبات

acetonitrile

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةUnder ice-cool
2. 2
   workup.STIRRINGAfter stirring for 1 hour
3. 3
   workup.DISTILLATIONthe solvent was distilled off under reduced pressure
4. 4
   workup.ADDITIONdiluted with water
5. 5
   استخلاصfollowed by extraction with ethyl acetate twice
6. 6
   تجفيفdried over anhydrous magnesium sulfate
7. 7
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure
8. 8
   أخرىthe residue was purified by silica gel column chromatography

الإجراء التجريبي

1.04 g of 2,4-diaminotoluene, 104 mg of 4-(dimethylamino)pyridine and 4.9 ml of N,N-diisopropyl-N-ethylamine were dissolved in 40 ml of acetonitrile. Under ice-cool stirring, 3.70 g of 4-(4-methylpiperazin-1-ylmethyl)-3-trifluoromethylbenzoyl chloride dihydrochloride (Reference Example 2) was added by four portions. After stirring for 1 hour, the solvent was distilled off under reduced pressure and diluted with water. The reaction solution was alkalified with an aqueous saturated sodium hydrogen carbonate solution, followed by extraction with ethyl acetate twice, and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography to obtain 2.56 g of the objective compound as a pale brown amorphous.

المصدر