HRID2059788
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
To a solution of 4-methyl-N-[4-(4-methyl-piperazin-1-ylmethyl)-3-trifluoromethylphenyl]-3-trimethylsilanylethynyl-benzamide (2.0 g, 4.1 mmol) in THF (15 mL) was added 5 mL of TBAF in THF (1.0M). After stirring at rt for 1 h, the mixture was partitioned between H2O and EtOAc. The combined organic layers were dried over Na2SO4, filtered, and then concentrated on a rotavap and the residue was purified on a silica gel column (eluent: 10% MeOH in CH2Cl2, MeOH was presaturated with ammonia gas) to give the desired product as a light yellow solid in 78% yield (1.33 g).
WORKUP
后处理
- customthe mixture was partitioned between H2O and EtOAc
- dry with materialThe combined organic layers were dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated on a rotavap
- customthe residue was purified on a silica gel column (eluent: 10% MeOH in CH2Cl2, MeOH was presaturated with ammonia gas)