HRID2079988
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
A mixture of the resulting quinoline-6-carboxylic acid 4-benzyloxy-benzylamide (310 mg, 0.84 mmol), 2,4-bis(4-methoxyphenyl)-1,3-dithia-2,4-diphosphetane-2,4-disulphide (Lawesson's reagent) (1.4 g, 3.4 mmol) and tetrahydrofuran (10 mL) was refluxed for 1 hour. After cooling, the solvent was evaporated in vacuo, dichloromethane was added to the residue, which was purified by NH silica gel column chromatography (hexane:ethyl acetate=1:1), and the title compound (55 mg, 0.14 mmol, 17%) was obtained as a pale yellow solid.
WORKUP
后处理
- temperaturewas refluxed for 1 hour
- temperatureAfter cooling
- customthe solvent was evaporated in vacuo, dichloromethane
- additionwas added to the residue, which
- customwas purified by NH silica gel column chromatography (hexane:ethyl acetate=1:1)