반응 #86403

반응 방정식

2,6-dichloro-3,5-dimethoxy-phenylamine

triphosgene

→

title compound

수율 162.0%

2,4-Dichloro-3-isocyanato-1,5-dimethoxy-benzene

수율 162.0%

용매

dioxane

반응 조건

후처리

1. 1
   농축The reaction was concentrated
2. 2
   기타the residue was purified by flash chromatography on silica eluting with DCM

실험 절차

A mixture of 2,6-dichloro-3,5-dimethoxy-phenylamine (500 g, 2.25 mmol), triphosgene (335 mg, 1.12 mmol) and TEA (342 g, 3.38 mmol) in dioxane (15 mL) was heated to 130° C. for 2 hours under microwave. The reaction was concentrated and the residue was purified by flash chromatography on silica eluting with DCM to obtain the title compound (450 mg, yield: 80%). 1H-NMR (400 MHz, CDCl3) δ 3.92 (s, 6H), 6.42 (s, 1H).

출처