تفاعل #2045112

معادلة التفاعل

2-methyl-5-chloropyridine

N-(tert-butyloxycarbonyl)piperazine

sodium tert-butoxide

BINAP

→

1-(tert-Butyloxycarbonyl)-4-(5-methylpyridin-2-yl)piperazine

المذيبات

toluene

diethyl ether

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةAfter cooling
2. 2
   غسيلthe mixture is washed three times with saturated sodium chloride solution
3. 3
   تجفيفdried over sodium sulphate
4. 4
   أخرىthe solvent is removed under reduced pressure
5. 5
   أخرىThe residue is purified by flash chromatography (cyclohexane/ethyl acetate 9:1)

الإجراء التجريبي

Under an atmosphere of argon, 2.50 g (19.6 mmol) of 2-methyl-5-chloropyridine and 4.38 g (23.5 mmol) of N-(tert-butyloxycarbonyl)piperazine are dissolved in 50 ml of absolute toluene. 2.26 g (23.5 mmol) of sodium tert-butoxide, 0.37 g (0.59 mmol) of BINAP and 0.36 g (0.39 mmol) of tris(dibenzylideneacetone)dipalladium are then added, and the mixture is heated at 70° C. for 12 h. After cooling, diethyl ether is added to the reaction mixture, the mixture is washed three times with saturated sodium chloride solution and dried over sodium sulphate and the solvent is removed under reduced pressure. The residue is purified by flash chromatography (cyclohexane/ethyl acetate 9:1).

المصدر