HRID1374802
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 the product from part (i) (0.4 g) in dichloromethane (10 ml) was added trifluoroacetic acid (2 ml), the reaction was stirred at room temperature overnight. The reaction was concentrated in vacuo and the residue dissolved/suspended in water. The pH was adjusted to 2 using 2M HCl(aq) and the solid which precipitated was isolated by filtration. This was purifed using reverse phase preparative HPLC (MeCN/NH3(aq) as eluent) to give a solid. The solid was suspended in water and the pH was adjusted to 2 using 2M HCl(aq), the solid was isolated by filtration, triturated with hexane and dried overnight at 40° C. under vaccum to give the title compound (0.15 g).
WORKUP
后处理
- concentrationThe reaction was concentrated in vacuo
- customthe solid which precipitated
- customwas isolated by filtration
- customto give a solid
- customthe solid was isolated by filtration
- customtriturated with hexane
- customdried overnight at 40° C. under vaccum