HRID1111403

反应详情

EQUATION

反应方程式

HRID 1111403 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.2 g of alpha-(2-furyl)-alpha-aminoacetonitrile hydrochloride was dissolved in 10 ml of pyridine, and with stirring at room temperature, 1.1 g of 3-methylisothiazole-4-carboxylic acid chloride was added dropwise. After the dropwise addition, the mixture was stirred for 1 hour, and distilled under reduced pressure to remove pyridine. The residue was dissolved in ethyl acetate, separated, washed with water, and dried over sodium sulfate. The ethyl acetate layer was distilled under reduced pressure to remove the solvent. The residue was purified by silica gel column chromatography. Elution with benzene-ethyl acetate gave 1.2 g (yield of the desired N-(alpha-cyanofurfuryl)-3-methylisothiazole-4-carboxylic acid amide.

WORKUP

后处理

  1. additionAfter the dropwise addition
  2. stirringthe mixture was stirred for 1 hour
  3. distillationdistilled under reduced pressure
  4. customto remove pyridine
  5. dissolutionThe residue was dissolved in ethyl acetate
  6. customseparated
  7. washwashed with water
  8. dry with materialdried over sodium sulfate
  9. distillationThe ethyl acetate layer was distilled under reduced pressure
  10. customto remove the solvent
  11. customThe residue was purified by silica gel column chromatography
  12. washElution with benzene-ethyl acetate