HRID636693
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 cooled and stirred suspension of protected 2-amino-3-benzoyl-6-benzyloxycarbonyl-4,5,6,7-tetrahydrothieno[2,3-c]pyridine (0.01 mol) in acetic acid (2 mL), as prepared in Example 7, was added a solution of HBr (33%) in acetic acid (10 mL). After stirring at room temperature for 4 h (TLC control), n-hexane was added and the resulting suspension was evaporated under vacuum to give a solid which was dissolved in water (10 mL) and neutralized with NAOH (5% solution). The precipitated solid was chromatographed on a silica gel column eluting with an ethyl acetate and petroleum ether mixture to give 2-amino-3-benzoyl4,5,6,7-tetrahydrothieno[2,3-c]pyridine.
WORKUP
后处理
- temperatureTo a cooled
- customas prepared in Example 7
- additionwas added
- customthe resulting suspension was evaporated under vacuum
- customto give a solid which
- customThe precipitated solid was chromatographed on a silica gel column
- washeluting with an ethyl acetate and petroleum ether mixture