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
CONDITIONS
反应条件
- 温度
- 25 °C
PROCEDURE
实验过程
A solution of (5-methylsulfanylmethyl-pyrazin-2-yl)-carbamic acid tert-butyl ester (0.45 g, 1.762 mmol) in methylene chloride (18 mL) was treated with trifluoroacetic acid (1.4 mL, 18.172 mmol) and then was stirred at 25° C. for 2 h 15 min. The reaction solution was then treated with a second aliquot of trifluoroacetic acid (0.7 mL, 9.086 mmol) and was stirred at 25° C. for 5 h. At this time, the reaction mixture was concentrated in vacuo. Biotage chromatography (FLASH 40S, Silica, 1/9 methanol/methylene chloride with 0.1% ammonium hydroxide) afforded 5-methylsulfanylmethyl-pyrazin-2-ylamine (276.1 mg, quant.) as a white solid: mp 102.0–102.7° C.; EI-HRMS m/e calcd for C6H9N3S (M+) 155.0517, found 155.0516.
WORKUP
后处理
- stirringwas stirred at 25° C. for 5 h
- concentrationAt this time, the reaction mixture was concentrated in vacuo