HRID731530

反应详情

EQUATION

反应方程式

HRID 731530 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The product from step (g) (0.3 g) was suspended in a mixture of dioxan (50 ml) and conc.HCl (1 ml). Water (1 ml) was added and the resultant solution heated at 60° C. for 12 hours. Allowed to stand over weekend. Solvents removed in vacuo and residue taken up in water. Yellow precipitate collected by filtration and washed with water. Purified using prep. Hplc Acetonitrile: 0.1% ammonium acetate (90:10 to 95:5) over 25 minutes to give 0.063 g of the desired product. 22% yield.

WORKUP

后处理

  1. waitAllowed to stand over weekend
  2. customSolvents removed in vacuo and residue
  3. filtrationYellow precipitate collected by filtration
  4. washwashed with water
  5. customPurified