HRID2423489

反应详情

EQUATION

反应方程式

HRID 2423489 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
64 °C

PROCEDURE

实验过程

A solution of 2,4-dichloro-3-pyridinecarbaldehyde oxime (1.88 g, 9.9 mmol) in DMF (7.9 mL) was stirred as N-chlorosuccinimide (1.32 g, 9.9 mmol) was added. The solution was stirred in a 64° C. oil bath for 1 hour then allowed to cool to room temperature. The solution was poured onto ice. The solution was extracted with ether and the organic layer was washed with brine, dried with MgSO4, filtered and concentrated to yield 2,4-dichloro-N-hydroxy-3-pyridinecarboximidoyl chloride (1.94 g, 87%). 1H NMR (400 MHz, DMSO-d6): δ 12.89 (s, 1H), 8.52 (d, J=5 Hz, 1H), 7.81 (d, J=5 Hz, 1H).

WORKUP

后处理

  1. additionwas added
  2. temperatureto cool to room temperature
  3. additionThe solution was poured onto ice
  4. extractionThe solution was extracted with ether
  5. washthe organic layer was washed with brine
  6. dry with materialdried with MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated