반응 #705141

ord-f846fad7421d48f8af11cbadf2235352

반응 방정식

O
water
[H-].[Na+]
sodium hydride
N#CCc1c(Cl)cccc1Cl
2,6-dichlorophenylacetonitrile
Nc1nc(Nc2ccccc2)ncc1C=O
4-amino-2-phenylamino-pyrimidine-5-carboxaldehyde
Nc1nc(Nc2ccccc2)ncc1C=O
4-Amino-2-phenylamino-pyrimidine-5-carboxaldehyde
Nc1nc2nc(Nc3ccccc3)ncc2cc1-c1c(Cl)cccc1Cl
title compound
수율 68.4%
Nc1nc2nc(Nc3ccccc3)ncc2cc1-c1c(Cl)cccc1Cl
6-(2, 6-Dichlorophenyl)-N2 -phenyl-pyrido [2, 3-d]-pyrimidine-2,7-diamine
수율 68.4%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The reaction was refluxed for 4 hours
  2. 2
    온도cooled
  3. 3
    추출extracted several times with dichloromethane
  4. 4
    세척washed with saturated sodium chloride
  5. 5
    건조dried with magnesium sulfate
  6. 6
    농축concentrated in vacuo
  7. 7
    세척The residue was washed with diethyl ether

실험 절차

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+.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05952342uspto-grants-1999_09