HRID1374802

反应详情

EQUATION

反应方程式

HRID 1374802 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. concentrationThe reaction was concentrated in vacuo
  2. customthe solid which precipitated
  3. customwas isolated by filtration
  4. customto give a solid
  5. customthe solid was isolated by filtration
  6. customtriturated with hexane
  7. customdried overnight at 40° C. under vaccum