HRID1086728

反应详情

EQUATION

反应方程式

HRID 1086728 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Valeryl chloride (0.2 ml, 1.98 mmole) was added dropwise to a stirred, ice cold solution of 3-{1-[(cis-4-benzyloxycarbonylcyclohexyl)carbamoyl]cyclopentyl}-2-(4-hydroxybutyl)propanoic acid t-butyl ester (0.7 g, 1.32 mmole) in dry pyridine (5 ml). The mixture was allowed to stand overnight at room temperature and ice was added, the pH was adjusted to 3 by the addition of 2N hydrochloric acid and the mixture was extracted with diethyl ether. The organic extract was dried (Na2SO4) and evaporated to give a gum which was chromatographed on silica eluting with hexane containing increasing proportions of diethyl ether to give the title product as a gum (. . . g . . . %). Found: C,70.06; H,8.91; N,2.58. C36H55NO7 requires C,70.44; H,9.03; N,2.28%.

WORKUP

后处理

  1. additionice was added
  2. extractionthe mixture was extracted with diethyl ether
  3. extractionThe organic extract
  4. dry with materialwas dried (Na2SO4)
  5. customevaporated
  6. customto give a gum which
  7. customwas chromatographed on silica eluting with hexane containing
  8. temperatureincreasing proportions of diethyl ether