HRID2286054

反应详情

EQUATION

反应方程式

HRID 2286054 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

3,4-Dihydro-2H-pyran (272 g.) was added dropwise at 40° C. with stirring to a mixture of 7-hydroxyheptanenitrile (284 g.) and concentrated hydrochloric acid (10 drops). The temperature was allowed to rise to 65° C. and was maintained at this level for one hour. The solution was cooled and benzene (500 ml.) was added. The solution was washed with aqueous sodium bicarbonate and then water, and dried over sodium sulphate. The solvent was removed in vacuo, and the residue distilled under reduced pressure to give 7-(2-tetrahydropyranyloxy)heptanenitrile (411 g.), b.p. 100°-130° C./0.1 mm.Hg, nD25 1.455.

WORKUP

后处理

  1. customto rise to 65° C.
  2. temperaturewas maintained at this level for one hour
  3. temperatureThe solution was cooled
  4. washThe solution was washed with aqueous sodium bicarbonate
  5. dry with materialwater, and dried over sodium sulphate
  6. customThe solvent was removed in vacuo
  7. distillationthe residue distilled under reduced pressure