HRID649038
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
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
- washthe mixture was washed with water
- extractionwith 6 ml of N sodium hydroxide, and was extracted with methylene chloride
- customThe organic phases were dried
- concentrationconcentrated to dryness
- customthe residue was chromatographed over silica
- washElution
- additionwith a mixture of hexane and ethyl acetate (8-2)