HRID1947858
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- concentrationThe reaction mixture was concentrated in vacuo
- customthe residue was purified on an Isco Combiflash
- washeluting with 50 to 90% EtOAc in heptane