HRID731971

反应详情

EQUATION

反应方程式

HRID 731971 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

This compound was prepared in a manner analogous to that set forth in Step B of Example 1, using 25 grams (0.093 mole) of 2,6-dichloro-4-phenylmethoxyphenol (known compound), 19.5 grams (0.10 mole) of 4-bromobutyl acetate and 19.4 grams (0.14 mole) of potassium carbonate in 400 mL of DMF, differing in that the reaction mixture was warmed to 80 C., where it was maintained prior to work-up. The crude reaction product was purified with column chromatography on silica gel using 1:1 methylene chloride:hexane as an eluant. The appropriate fractions were combined and concentrated under reduced pressure, yielding 33.1 grams of compound the subject compound. The NMR spectrum was consistent with the proposed structure.

WORKUP

后处理

  1. customThis compound was prepared in a manner analogous to that set forth in Step B of Example 1
  2. temperaturewas warmed to 80 C
  3. temperature, where it was maintained
  4. customThe crude reaction product
  5. customwas purified with column chromatography on silica gel using 1:1 methylene chloride
  6. concentrationconcentrated under reduced pressure