Реакция #417993

ord-8142f9101be64e36b2c5e5f70a56c150

Уравнение реакции

Clc1cc(I)ccn1
2-chloro-4-iodopyridine
CC[O-].[Na+]
sodium ethoxide
CCOc1cc(I)ccn1
2-Ethoxy-4-iodopyridine

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураat reflux for 12 h
  2. 2
    ДругоеThe solvent is evaporated in vacuo
  3. 3
    Другоеthe residue is partitioned between water and DCM
  4. 4
    СушкаThe organic layer is dried over sodium sulphate
  5. 5
    Другоеthe solvent is removed in vacuo
  6. 6
    ДругоеThe crude product is purified by column chromatography (silica gel; DCM/MeOH gradient 100/0→96/4)

Методика

To 2.00 g (8.35 mmol) 2-chloro-4-iodopyridine in 15 mL ethanol are added 3.4 mL (9.2 mmol) sodium ethoxide and stirred at reflux for 12 h. The solvent is evaporated in vacuo and the residue is partitioned between water and DCM. The organic layer is dried over sodium sulphate and the solvent is removed in vacuo. The crude product is purified by column chromatography (silica gel; DCM/MeOH gradient 100/0→96/4).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08877754B2uspto-grants-2014_11