Реакция #2161261

ord-e56fe79a6b7b4ec4b73f4b164cfe0b89

Уравнение реакции

Clc1cc(Cl)nc(Cl)n1
2,4,6-trichloropyrimidine
CCNCC
diethylamine
CCN(CC)CC
triethylamine
CCN(CC)c1cc(Cl)nc(Cl)n1
(2,6-Dichloro-pyrimidin-4-yl)-diethyl-amine

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    КонцентрированиеThe mixture was then concentrated
  2. 2
    workup.ADDITION25 mL of CH2Cl2 and 25 mL of water were added
  3. 3
    ДругоеThe organic layer was separated
  4. 4
    Экстракцияthe aqueous layer was extracted by additional amount of dichloromethane (2×10 mL)
  5. 5
    Сушкаdried over anhydrous Na2SO4
  6. 6
    Концентрированиеconcentrated
  7. 7
    ДругоеColumn chromatography on silica gel afforded 1.48 g (62%) of L as colorless solid

Методика

To a stirred solution of 2.0 g (10.90 mmols) of 2,4,6-trichloropyrimidine in 25 mL of anhydrous ethanol at 0° C., was added drop wise a solution 0.79 g (10.90 mmols) of diethylamine in 5 mL of ethanol. This was followed by the addition of 2.3 mL (16.35 mmols) of triethylamine and the mixture was stirred for further 30 min. The mixture was then concentrated and 25 mL of CH2Cl2 and 25 mL of water were added. The organic layer was separated and the aqueous layer was extracted by additional amount of dichloromethane (2×10 mL) and the extracts were combined, dried over anhydrous Na2SO4 and concentrated. Column chromatography on silica gel afforded 1.48 g (62%) of L as colorless solid.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07919487B2uspto-grants-2011_04