Реакция #2146762

ord-fb3ec38cabbc4589a151f2ca6ca6887b

Уравнение реакции

[O-][n+]1ccc2cc(F)c(Cl)cc2c1
7-Chloro-6-fluoro-isoquinoline 2-oxide
O=P(Cl)(Cl)Cl
POCl3
Fc1cc2ccnc(Cl)c2cc1Cl
title compound
Fc1cc2ccnc(Cl)c2cc1Cl
1,7-Di-chloro-6-fluoro-isoquinoline

Реагенты

Нет

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураat reflux for 4 h
  2. 2
    workup.ADDITIONit was poured on ice
  3. 3
    ЭкстракцияThe aqueous solution was extracted three times with dichloromethane
  4. 4
    СушкаThe combined organic layers were dried with MgSO4
  5. 5
    Другоеevaporated

Методика

2.6 g (12.0 mmol) of 7-Chloro-6-fluoro-isoquinoline 2-oxide (4) were heated in 40 ml of POCl3 at reflux for 4 h. After the mixture has cooled down to room temperature, it was poured on ice. The aqueous solution was extracted three times with dichloromethane. The combined organic layers were dried with MgSO4 and evaporated to yield 2.91 g of the title compound, which was used without further purification. Rt=2.34 min (Method A). Detected mass: 216.0/218.0 (M+H+).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08278294B2uspto-grants-2012_10