HRID1776461

反应详情

EQUATION

反应方程式

HRID 1776461 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

(S)-3,5-dichloro-4-(2-(3-(cyclopropylmethoxy)-4-(difluoromethoxy)phenyl)-2-hydroxyethyl)pyridine 1-oxide (1.5 g, 3.57 mmol), and DMAP (0.436 g, 3.57 mmol) were dissolved in DCM (50 ml), and 4-nitrophenyl carbonochloridate (0.863 g, 4.28 mmol) was added portion wise. The mixture was stirred at RT overnight. After 18 hours, the solvent was evaporated and the crude purified by silica gel flash chromatography (petroleum ether:EtOAc 3:7) affording (S)-3,5-dichloro-4-(2-(3-(cyclopropylmethoxy)-4-(difluoromethoxy)phenyl)-2-((4-nitrophenoxy)carbonyloxy)-ethyl)pyridine 1-oxide (1.609 g, 2.75 mmol, 77% yield, MS/ESI+ 585 [MH]+).

WORKUP

后处理

  1. waitAfter 18 hours
  2. customthe solvent was evaporated
  3. customthe crude purified by silica gel flash chromatography (petroleum ether:EtOAc 3:7)