Реакция #3543

ord-32214df9473647ba998abcb895c010fa

Уравнение реакции

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
Выход 68.4%
Nc1nc2nc(Nc3ccccc3)ncc2cc1-c1c(Cl)cccc1Cl
6-(2,6-Dichlorophenyl)-N2 -phenyl-pyrido[2,3-d]-pyrimidine-2,7-diamine
Выход 68.4%

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураThe reaction was refluxed for 4 hours
  2. 2
    Температураcooled
  3. 3
    Экстракцияextracted several times with dichloromethane
  4. 4
    Промывкаwashed with saturated sodium chloride
  5. 5
    Сушкаdried with magnesium sulfate
  6. 6
    Концентрированиеconcentrated in vacuo
  7. 7
    ПромывкаThe residue was washed with diethyl ether

Методика

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+.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05733913uspto-grants-1998_03