HRID580045

反应详情

EQUATION

反应方程式

HRID 580045 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of 5 g (0.023 m) of 4-(2-keto-1-benzimidazolinyl)piperidine, 7.65 g (0.023 m) of 2-(6,11-dihydro-11-oxodibenz[b,e]oxepin-2-yl)ethanol methanesulfonate of Example 1 and 3.17 g (0.023 m) of K2CO3 in 30 ml of absolute ethanol and 60 ml of methanol was refluxed overnight (about 16 hours). The reaction mixture was diluted with 800 ml of ethyl acetate, filtered and evaporated in vacuo. The residue was recrystallized from methanol to give after drying at 100° C. in vacuo, 5.78 g (56%) of 4-(2-keto-1-benzimidazolinyl)-1-[2-(6,11-dihydro-11-oxodibenz[b,e]oxepin-2-yl)ethyl]piperidine, m.p. 116°-120° C.

WORKUP

后处理

  1. temperaturewas refluxed overnight (about 16 hours)
  2. filtrationfiltered
  3. customevaporated in vacuo
  4. customThe residue was recrystallized from methanol
  5. customto give
  6. dry with materialafter drying at 100° C. in vacuo, 5.78 g (56%) of 4-(2-keto-1-benzimidazolinyl)-1-[2-(6,11-dihydro-11-oxodibenz[b,e]oxepin-2-yl)ethyl]piperidine, m.p. 116°-120° C.