HRID2246711

反应详情

EQUATION

反应方程式

HRID 2246711 的结构方程式

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

Thiosalicylic acid was added to a solution of the product from Example 1 part (iv) (474 mg) in trifluoroacetic acid (10 ml) was added thiosalicylic acid (351 mg) and the resulting suspension was heated to 60° C. for 4 hours. The mixture was concentrated in vacuo and the residue dissolved in EtOAc and washed with NaHCO3 (aq), brine, dried (MgSO4) and evaporated to give crude material. Purification by column chromatography (50% EtOAc/hexane as eluent) gave the sub-title compound (0.13 g).

WORKUP

后处理

  1. concentrationThe mixture was concentrated in vacuo
  2. dissolutionthe residue dissolved in EtOAc
  3. washwashed with NaHCO3 (aq), brine
  4. dry with materialdried (MgSO4)
  5. customevaporated
  6. customto give crude material
  7. customPurification by column chromatography (50% EtOAc/hexane as eluent)