HRID1947858

反应详情

EQUATION

反应方程式

HRID 1947858 的结构方程式

PROCEDURE

实验过程

A solution of 4-(bromomethyl)-2-chloro-1-nitrobenzene (Compound 104D, 2.9 g, 12 mmol) in triethyl phosphite (2.6 mL, 15 mmol) was stirred at 120° C. for 16 h under nitrogen. The reaction mixture was concentrated in vacuo and the residue was purified on an Isco Combiflash eluting with 50 to 90% EtOAc in heptane to afford the title compound. MS (ES+): m/z: 308.0416 [MH+]. HPLC: tR=1.33 min (UPLC TOF MS: polar—3 min).

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. customthe residue was purified on an Isco Combiflash
  3. washeluting with 50 to 90% EtOAc in heptane