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
Methyl indole-2-carboxylate (0.15 g) was dissolved in DMF and sodium hydride (41 mg) was added in a single portion. The reaction was stirred for 1 hour, then 3,4-dichlorobenzenesulphonyl chloride (0.25 g) was added in a single portion. Stirring was continued for a further 2 hours and then the reaction was quenched by the addition of water. The reaction mixture was partitioned between water and ethyl acetate. Combined organic extracts were dried (MgSO4) and concentrated in vacuo and the residue purified by column chromatography using isohexane-5% ethyl acetate as eluent to give the desired end product as a solid (51%). NMR δ (CDCl3) 3.96 (s, 3H), 7.22-8.20 (m, 8H); M/z (+) 384 (MH+), 352, 175.
WORKUP
后处理
- stirringStirring
- waitwas continued for a further 2 hours
- customthe reaction was quenched by the addition of water
- customThe reaction mixture was partitioned between water and ethyl acetate
- dry with materialCombined organic extracts were dried (MgSO4)
- concentrationconcentrated in vacuo
- customthe residue purified by column chromatography