HRID365369

反应详情

EQUATION

反应方程式

HRID 365369 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a 50 ml round bottomed flask equipped with condenser and nitrogen inlet were added 370 mg (1.69 mmol) 5-(2-chloroethyl)oxindole, 400 mg (1.69 mmol) N-(1-naphthyl)piperazine hydrochloride, 200 mg (1.69 mmol) sodium carbonate, 2 mg sodium iodide, and 50 ml methylisobutylketone. The reaction was refluxed 24 hours, cooled, and evaporated. The residue was taken up in ethyl acetate, washed with water and brine, dried over sodium sulfate, and evaporated. The residue was chromatographed on silica gel with ethyl acetate, and the product fractions collected and evaporated to give a foam. The foam was dissolved in ether, treated with hydrochloric acid gas, and the precipitate collected, washed with ether, and dried to afford a white solid, m.p. 303°-305° C., 603 mg (84%).

WORKUP

后处理

  1. customTo a 50 ml round bottomed flask equipped with condenser and nitrogen inlet
  2. temperatureThe reaction was refluxed 24 hours
  3. temperaturecooled
  4. customevaporated
  5. washwashed with water and brine
  6. dry with materialdried over sodium sulfate
  7. customevaporated
  8. customThe residue was chromatographed on silica gel with ethyl acetate
  9. customthe product fractions collected
  10. customevaporated
  11. customto give a foam
  12. customthe precipitate collected
  13. washwashed with ether
  14. customdried
  15. customto afford a white solid, m.p. 303°-305° C., 603 mg (84%)