HRID1896531
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
1-[(4-Methoxybenzyl)amino]-7-[4-(trifluoromethyl)phenyl][1]benzothieno[3,2-c]pyridine-4-carbonitrile was placed in a flask cooled to 0° C. before conc. H2SO4 (excess) was added dropwise under vigorous stirring. The final mixture was warmed to room temperature and, after 1 h, poured into THF/EtOAc and aqueous NaHCO3 previously saturated with NaCl solid. After separation of the organic phase, the aqueous phase was extracted again with THF/EtOAc, and the combined organic phases were dried over MgSO4 and filtered. After evaporation of the organic solvents, the crude material was purified by a wash with Et2O to provide the title compound as a yellow solid.
WORKUP
后处理
- additionwas added dropwise under vigorous stirring
- customAfter separation of the organic phase
- extractionthe aqueous phase was extracted again with THF/EtOAc
- dry with materialthe combined organic phases were dried over MgSO4
- filtrationfiltered
- customAfter evaporation of the organic solvents
- customthe crude material was purified by
- washa wash with Et2O