HRID1577505

反应详情

EQUATION

反应方程式

HRID 1577505 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 5-(dimethylaminomethyl)-4-methyl-2-furanmethanol (1.35 g) and potassium tert-butoxide (0.9 g) in dry dimethylformamide (3 ml) at 0° was treated with a solution of 2-chloropropylamine, hydrochloride (0.4 g) in dry dimethylformamide (2 ml). After 20 minutes at ambient temperature, the mixture was quenched with oxalic acid (2 g) and the solvent removed in vacuo. Excess anhydrous sodium carbonate was added and the product extracted into chloroform. The chloroform extract was purified by filtration and the solvent evaporated in vacuo. The residue was purified by column chromatography (silica, methanol: 0.88 ammonia 19:1) affording the title compound (0.1 g).

WORKUP

后处理

  1. customthe mixture was quenched with oxalic acid (2 g)
  2. customthe solvent removed in vacuo
  3. additionExcess anhydrous sodium carbonate was added
  4. extractionthe product extracted into chloroform
  5. extractionThe chloroform extract
  6. filtrationwas purified by filtration
  7. customthe solvent evaporated in vacuo
  8. customThe residue was purified by column chromatography (silica, methanol: 0.88 ammonia 19:1)