HRID59727
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 methyl 1-(4-nitrophenylsulfonyl)-1H-pyrrole-2-carboxylate (Int. 4) (550 mg, 1.773 mmol) in pyridine (25 ml), lithium iodide (1661 mg, 12.41 mmol) was added and the resulting mixture was refluxed for 8 hours. The solution was concentrated under vacuum and the crude was dissolved in DCM (150 ml) and washed with 1N HCl (50 ml×2) and then with brine (50 ml); the organic layer was dried over sodium sulfate and the solvent was removed affording 1-(4-nitrophenylsulfonyl)-1H-pyrrole-2-carboxylic acid (Int. 5) (433 mg, 1.462 mmol).
WORKUP
后处理
- temperaturethe resulting mixture was refluxed for 8 hours
- concentrationThe solution was concentrated under vacuum
- dissolutionthe crude was dissolved in DCM (150 ml)
- washwashed with 1N HCl (50 ml×2)
- dry with materialthe organic layer was dried over sodium sulfate
- customthe solvent was removed