反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
2.37 g of {3-[2-(4-chlorophenyl)imidazo[1,2-a]pyridin-6-yl]phenyl}methanol are suspended in 80 ml of dichloromethane; 4.26 ml of a 5N solution of hydrochloric acid in 2-propanol are added thereto, dropwise and with stirring, and the mixture is stirred at ambient temperature for 2 hours. The reaction mixture is then concentrated under reduced pressure. The residue solid is taken up with diisopropyl ether and the precipitate is recovered by filtration, washed with dichloromethane and then ethyl acetate and filter-dried. The solid is dissolved at ambient temperature with the minimum amount of methanol and then reprecipitated using diisopropyl ether. The precipitate is recovered by filtration and dried in an oven under reduced pressure at 60° C. 2.23 g of pale yellow solid are obtained. Mp=244-246° C. 1H NMR (DMSO-d6, δ in ppm): 4.59 (s, 2H); from 7.36 to 7.55 (m, 2H); from 7.58 to 7.74 (m, 4H); 7.96 (d, J=9.4 Hz, 1H); 8.05 (m, J=8.7 Hz, 2H); 8.14 (dd, J=9.3 Hz and 1.7 Hz, 1H); 8.70 (s, 1H); 9.15 (m, 1H). M+H=335.
WORKUP
后处理
- stirringthe mixture is stirred at ambient temperature for 2 hours
- concentrationThe reaction mixture is then concentrated under reduced pressure
- filtrationthe precipitate is recovered by filtration
- washwashed with dichloromethane
- dry with materialethyl acetate and filter-dried
- dissolutionThe solid is dissolved at ambient temperature with the minimum amount of methanol
- customreprecipitated
- filtrationThe precipitate is recovered by filtration
- customdried in an oven under reduced pressure at 60° C