HRID23411
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 6-methoxy-3-thiocyanato-1H-indole (0.336 g, 1.64 mmole) and methyl iodide (0.700 g, 4.93 mmole) in methanol (10 ml) was added potassium hydroxide solution (0.164 ml, 10N) at 0° C. The reaction mixture was stirred for 1 h at room temperature. Silica gel (5 g) was added to the reaction mixture and the solvent was removed under reduced pressure. The residue was purified on a column of silica gel, eluting the product with mixtures of ethyl acetate:hexane (1:9 to 1:1). The first product which was eluted was the desired 6-methoxy-3-methylsulfanyl-1H-indole (0.120 g, 37% yield) followed by 6-methoxy-1H-indole-3-thiol (0.126 g). Step 3
WORKUP
后处理
- additionSilica gel (5 g) was added to the reaction mixture
- customthe solvent was removed under reduced pressure
- customThe residue was purified on a column of silica gel
- washeluting the product with mixtures of ethyl acetate:hexane (1:9 to 1:1)
- washThe first product which was eluted