HRID2182212

反应详情

EQUATION

反应方程式

HRID 2182212 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Combine 1-bromo-2,4-difluorobenzene (1.00 g, 5.18 mmol), N,N′-dimethylethylenediamine (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-difluorophenyl)-N,N′-dimethylethylenediamine.

WORKUP

后处理

  1. temperatureHeat at 110° for 18 h
  2. temperatureto cool
  3. extractionextract with 1N HCl
  4. extractionextract with CH2Cl2
  5. customDry
  6. concentrationconcentrate
  7. custompurify by PLC