HRID1008483
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 140 °C
PROCEDURE
实验过程
A mixture of 10 g of 1b, 31 g of phenol and 4 g of KOH was heated at 140° C. for 2 hours. After cooling to room temperature aqueous 3N NaOH was added and the mixture was extracted with dichloromethane. The dichloromethane extract was washed with aqueous 2N NaOH, washed with water, dried (MgSO4) and concentrated to yield 12.2 g of 1c. 1H-NMR 200 MHz (CDCl3) δ: 7.1-7.6 (6H, m), 7.70 (1H, dd, J=9 Hz and J=2 Hz), 7.95-8.10 (2H, m), 8.31 (1H, d, J=9 Hz).
WORKUP
后处理
- additionwas added
- extractionthe mixture was extracted with dichloromethane
- extractionThe dichloromethane extract
- washwas washed with aqueous 2N NaOH
- washwashed with water
- dry with materialdried (MgSO4)
- concentrationconcentrated