HRID2205857

反应详情

EQUATION

反应方程式

HRID 2205857 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
2.5 °C

PROCEDURE

实验过程

N-(2-chloro-5-iodopyridin-4-yl)-N-(methylsulfonyl)methanesulfonamide (13) (1.1 g) was stirred with THF (6.8 mL) and 10% sodium hydroxide (6.8 mL) at room temperature overnight. The THF was evaporated and the aqueous was brought to pH about 5 with 10% citric acid solution. Product was deposited—the mixture was cooled at 0-5° C. for 0.5 h and the product filtered off. It was washed with a little water and dried over sodium hydroxide in a vacuum desiccator to give the title compound (772 mg, 83%). 1H-NMR (500 MHz, DMSO-d6): 3.29 (s, 3H), 7.42 (s, 1H), 8.66 (s, 1H).

WORKUP

后处理

  1. customThe THF was evaporated
  2. filtrationthe product filtered off
  3. washIt was washed with a little water
  4. dry with materialdried over sodium hydroxide in a vacuum desiccator