HRID1186441
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
Tetrahydrofuran (6 mL) was added to tert-butylamine (220 mg, 3.0 mmol), and 2,2,2-trifluoroethanesulfonyl chloride (300 mg, 1.6 mmol) was slowly added dropwise thereto. The mixture was stirred at room temperature for 30 minutes, and the solvent was evaporated off under reduced pressure. To the residue, trifluoroacetic acid (3.3 mL) was added and the mixture was stirred at room temperature for 15 hours. The solvent was evaporated off under reduced pressure, and purification by silica gel column chromatography (chloroform/methanol=100/0 to 5/1) was performed to give 2,2,2-trifluoroethanesulfonamide (Compound GC) (66 mg, yield: 25%).
WORKUP
后处理
- additionwas slowly added dropwise
- customthe solvent was evaporated off under reduced pressure
- additionTo the residue, trifluoroacetic acid (3.3 mL) was added
- stirringthe mixture was stirred at room temperature for 15 hours
- customThe solvent was evaporated off under reduced pressure, and purification by silica gel column chromatography (chloroform/methanol=100/0 to 5/1)