Реакция #2175419

ord-46127ada5fed45d7ad63de91832aeff4

Уравнение реакции

Fc1ccc(Br)c(F)c1
1-bromo-2,4-difluorobenzene
CNCCNC
N,N′-dimethyl-ethylenediamine
CC(C)(C)[O][Na]
NaO-t-Bu
CNCCN(C)c1ccc(F)cc1F
N-(2,4-difluoro-phenyl)-N,N′-dimethylethylenediamine

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураHeat at 110° for 18 h
  2. 2
    Температураto cool
  3. 3
    Экстракцияextract with 1N HCl
  4. 4
    Экстракцияextract with CH2Cl2
  5. 5
    ДругоеDry
  6. 6
    Концентрированиеconcentrate
  7. 7
    Другоеpurify by PLC

Методика

Combine 1-bromo-2,4-difluorobenzene (1.00 g, 5.18 mmol), N,N′-dimethyl-ethylenediamine (2.74 g, 31.1 mmol), NaO-t-Bu (0.70 g, 7.2 mmol), Pd(dba)2 (0.060 g, 0.10 mmol) and (±)-BINAP (0.19 g, 0.31 mmol) in toluene (10 ml). Heat at 110° for 18 h, allow to cool, and extract with 1N HCl. Basify the aqueous solution with NaOH and extract with CH2Cl2. Dry, concentrate, and purify by PLC to give N-(2,4-difluoro-phenyl)-N,N′-dimethylethylenediamine.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: USRE044205E1uspto-grants-2013_05