تفاعل #320723

ord-5ab4ecf8d0ed43bfb4b6684e10f91833

معادلة التفاعل

O=S(=O)([O-])OOS(=O)(=O)[O-].[K+].[K+]
Potassium persulfate
CSc1nccc(-c2c(-c3ccccc3F)ncn2C2CCN(C)CC2)n1
4-(fluorophenyl)-1-(methyl-4-piperidinyl)-5-(2-methylthio-4-pyrimidinyl)imidazole
[NH4+].[OH-]
NH4OH
CN1CCC(n2cnc(-c3ccccc3F)c2-c2ccnc(S(C)=O)n2)CC1
title compound
CN1CCC(n2cnc(-c3ccccc3F)c2-c2ccnc(S(C)=O)n2)CC1
4-(Fluorophenyl)-1-(methyl-4-piperidinyl)-5-(2-methysulfinyl-4-pyrimidinyl)imidazole

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصextracted with CH2Cl2
  2. 2
    استخلاصThe organic extract
  3. 3
    غسيلwas washed with brine
  4. 4
    تجفيفdried (MgSO4)
  5. 5
    تركيزconcentrated
  6. 6
    أخرىThe residue was triturated with ethyl ether

الإجراء التجريبي

Potassium persulfate (3.2 g, 7.0 mmol) in water (75 mL) was added to a solution of 4-(fluorophenyl)-1-(methyl-4-piperidinyl)-5-(2-methylthio-4-pyrimidinyl)imidazole (2.7 g, 7.0 mmol) in glacial AcOH (150 mL). After stirring at ambient temperature for 72 h, the reaction mixture was neutralized by the portion-wise addition of concentrated aqueous NH4OH and extracted with CH2Cl2. The organic extract was washed with brine, dried (MgSO4) and concentrated. The residue was triturated with ethyl ether to afford the title compound as an off-white solid; yield 2.3 g (83%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05593991uspto-grants-1997_01