HRID1896531

反应详情

EQUATION

反应方程式

HRID 1896531 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionwas added dropwise under vigorous stirring
  2. customAfter separation of the organic phase
  3. extractionthe aqueous phase was extracted again with THF/EtOAc
  4. dry with materialthe combined organic phases were dried over MgSO4
  5. filtrationfiltered
  6. customAfter evaporation of the organic solvents
  7. customthe crude material was purified by
  8. washa wash with Et2O