تفاعل #3543

ord-32214df9473647ba998abcb895c010fa

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe reaction was refluxed for 4 hours
  2. 2
    درجة الحرارةcooled
  3. 3
    استخلاصextracted several times with dichloromethane
  4. 4
    غسيلwashed with saturated sodium chloride
  5. 5
    تجفيفdried with magnesium sulfate
  6. 6
    تركيزconcentrated in vacuo
  7. 7
    غسيلThe residue was washed with diethyl ether

الإجراء التجريبي

To a solution of 0.022 g 60% sodium hydride suspension in 2.00 mL of 2-ethoxyethanol was added 0.46 g of 2,6-dichlorophenylacetonitrile and 0.50 g of 4-amino-2-phenylamino-pyrimidine-5-carboxaldehyde from Example 72. The reaction was refluxed for 4 hours, cooled, poured into water, and extracted several times with dichloromethane. The dichloromethane washes were combined, washed with saturated sodium chloride, dried with magnesium sulfate, and concentrated in vacuo. The residue was washed with diethyl ether to give 0.61 g of the title compound, CIMS (1% NH3 in CH4): 410=M+ +C2H5, 382=M+ +H, 381=M+.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05733913uspto-grants-1998_03