反应详情

温度

150 °C

step 3—Anhydrous collidine (100 mL) was added to a dry flask containing 3-bromo-5-methoxy-benzonitrile (10.4 g, 49 mmol) and LiI (19.6 g, 3 equiv). The solution was heated under nitrogen to 150° C. overnight, cooled to RT, and poured into an ice cold 1 M HCl solution. The mixture was extracted with a 1:1 EtOAc/hexanes solution, washed with water, and dried (MgSO4). Concentration in vacuo afforded 8.7 g (89%) of 3-bromo-5-hydroxy-benzonitrile.

1. temperaturecooled to RT
2. extractionThe mixture was extracted with a 1:1 EtOAc/hexanes solution
3. washwashed with water
4. dry with materialdried (MgSO4)
5. concentrationConcentration in vacuo