HRID59727

反应详情

EQUATION

反应方程式

HRID 59727 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturethe resulting mixture was refluxed for 8 hours
  2. concentrationThe solution was concentrated under vacuum
  3. dissolutionthe crude was dissolved in DCM (150 ml)
  4. washwashed with 1N HCl (50 ml×2)
  5. dry with materialthe organic layer was dried over sodium sulfate
  6. customthe solvent was removed