HRID28445

反应详情

EQUATION

反应方程式

HRID 28445 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of supported triphenyl phosphine (6.55 g, 19.67 mmol) in CH2Cl2 at 0° C. was added iodine (4.99 g, 19.67 mmol) and imidazole (1.33 g, 19.67 mmol). The mixture was warmed to ambient temperature, stirred for 1 h and cooled to 0° C. for the dropwise addition of (R)-2,6-dimethyl heptan-1-ol in CH2Cl2 (5 mL). The mixture was allowed to reach ambient temperature and stirred for 1 h, at which time it was filtered through a pad of celite and the solids were washed with CH2Cl2. The filtrated was concentrated, and the crude product was purified via silica gel chromatography to give (R)-1-iodo-2,6-dimethyl heptane (2.44 g).

WORKUP

后处理

  1. customto reach ambient temperature
  2. stirringstirred for 1 h, at which time it
  3. filtrationwas filtered through a pad of celite
  4. washthe solids were washed with CH2Cl2
  5. concentrationThe filtrated was concentrated
  6. customthe crude product was purified via silica gel chromatography