تفاعل #575030

ord-8af2cc36434543c9bac5e719789ad607

معادلة التفاعل

ClCCl
dichloromethane
CCC1(c2ccccc2)C(=O)NC(=O)N(CCCCC(=O)Cl)C1=O
acid chloride
CCC1(c2ccccc2)C(=O)NC(=O)N(CCCCC(=O)Cl)C1=O
1-(4-chlorocarbonylbutyl)-5-ethyl-5-phenyl-2,4,6(1H,3H,5H)pyrimidinetrione
O=C(OCc1ccccc1)N1CCNCC1
benzyl 1-piperazinecarboxylate
CCN(CC)CC
triethylamine
CCC1(c2ccccc2)C(=O)NC(=O)N(CCCCC(=O)N2CCN(C(=O)OCc3ccccc3)CC2)C1=O
1-[4-(4-Benzyloxycarbonyl-1-piperazinylcarbonyl)butyl]-5-ethyl-5-phenyl-2,4,6(1H,3H,5H)pyrimidinetrione

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    غسيلThe mixture was washed with 10% hydrochloric acid solution (3×100 mL)
  2. 2
    غسيلwashed with saturated sodium chloride solution (100 mL)
  3. 3
    تجفيفdried over anhydrous magnesium sulfate
  4. 4
    ترشيحfiltered
  5. 5
    أخرىthe solvent removed
  6. 6
    أخرىThe residue was then chromatographed on SiO2
  7. 7
    أخرىto give a solid

الإجراء التجريبي

The acid chloride of step 3 (0.2 mole) in chloroform (75 mL) was added dropwise over 15 minutes to a mixture of benzyl 1-piperazinecarboxylate (6.0 g, 0.030 mole) and triethylamine (4.0 g, 0.04 mole) in chloroform (100 mL). This mixture was stirred at room temperature for 20 hrs, and dichloromethane was then added (300 mL). The mixture was washed with 10% hydrochloric acid solution (3×100 mL), washed with saturated sodium chloride solution (100 mL), dried over anhydrous magnesium sulfate, filtered, and the solvent removed. The residue was then chromatographed on SiO2 to give a solid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05298403uspto-grants-1994_03