HRID221365

反应详情

EQUATION

反应方程式

HRID 221365 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of cis-[3-(3-pyridin-4-yl-[1,2,4]oxadiazol-5-yl)cyclopentyl]methanol (Preparation 5, 40 mg, 0.116 mmol) in anhydrous THF (2 ml) was treated with sodium hydride (23 mg of a 60% dispersion in oil, 0.57 mmol) and tetrabutylammonium iodide (6 mg, 16 μmol). After stirring the mixture at rt for 10 min, 1-bromobutane (59 μl, 0.65 mmol) was introduced and stirring continued for 72 h. The solvent was removed in vacuo, the residue dissolved in CH2Cl2 (20 ml) and washed with water (2×5 ml). The organic phase was dried (MgSO4) and evaporated. Flash chromatography (IH-EtOAc, 7:3) afforded the title compound: RT=3.99 min, m/z (ES−)=302.3 [M+H]+.

WORKUP

后处理

  1. stirringstirring
  2. waitcontinued for 72 h
  3. customThe solvent was removed in vacuo
  4. dissolutionthe residue dissolved in CH2Cl2 (20 ml)
  5. washwashed with water (2×5 ml)
  6. dry with materialThe organic phase was dried (MgSO4)
  7. customevaporated