HRID389208
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
To the product from Step 2 (363 mg, 1.2 mmol) was added phosgene (20% solution in PhMe, 5.9 g, 11.97 mmol), and the mixture was heated to reflux for 2 hours. The solvent was then removed in vacuo to give crude 4′-bromo-2-isocyanato-3′-methoxybiphenyl-4-carbonitrile (394 mg, 1.2 mmol), which was then taken up in chlorobenzene (4 mL). To this mixture, AlCl3 (319 mg, 2.4 mmol) was added at RT. 1 N HCl (30 mL) was then added, which caused a grey precipitate to form. This was isolated by filtration and washed with DCM and MeOH to give the title compound. LRMS (M+H)+=329.0.
WORKUP
后处理
- temperaturethe mixture was heated
- temperatureto reflux for 2 hours
- customThe solvent was then removed in vacuo