HRID649038

反应详情

EQUATION

反应方程式

HRID 649038 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

40 ml of a solution of 45 (mmoles) of 2-chlorocarbonyl-1H-pyrrole in methylene chloride were added dropwise to a cold mixture of 4.3 ml of pyridine and 3.5 ml of methanol and the mixture was washed with water, then with 6 ml of N sodium hydroxide, and was extracted with methylene chloride. The organic phases were dried and concentrated to dryness and the residue was chromatographed over silica. Elution with a mixture of hexane and ethyl acetate (8-2) yielded 4.014 g of methyl 1H-pyrrole-2-carboxylate melting at ≃74° C.

WORKUP

后处理

  1. washthe mixture was washed with water
  2. extractionwith 6 ml of N sodium hydroxide, and was extracted with methylene chloride
  3. customThe organic phases were dried
  4. concentrationconcentrated to dryness
  5. customthe residue was chromatographed over silica
  6. washElution
  7. additionwith a mixture of hexane and ethyl acetate (8-2)