HRID2246711
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- concentrationThe mixture was concentrated in vacuo
- dissolutionthe residue dissolved in EtOAc
- washwashed with NaHCO3 (aq), brine
- dry with materialdried (MgSO4)
- customevaporated
- customto give crude material
- customPurification by column chromatography (50% EtOAc/hexane as eluent)